Category: 627-30-5

Reference of 627-30-5 ,Some common heterocyclic compound, 627-30-5, molecular formula is C3H7ClO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

The 4-CHLORO-7- (3-CHLOROPROPOXY)-6-METHOXYQUINAZOLINE used as a starting material was prepared as follows:- Ammonium formate (45 g) was added portionwise over 1.25 hours to a stirred mixture of 7-benzyloxy-6-methoxy-3,4-dihydroquinazolin-4-one (International Patent Application WO 02/16352, Example 1 thereof; 20 g), 10% palladium-on-carbon catalyst (3.3 g) and DMF (530 ml) and the reaction mixture was stirred for an additional 30 minutes. The catalyst was removed by filtration and the solvent was evaporated. There was thus obtained 7-hydroxy- 6-methoxy-3,4-dihydroquinazolin-4-one (8.65 g); NMR Spectrum: (DMSOD6) 3.9 (s, 3H), 7.0 (s, 1H), 7.45 (s, 1H), 7.9 (s, 1H). A mixture of the material so obtained, acetic anhydride (63 ml) and pyridine (7.5 ml) was heated to 100C for 4.5 hours. The resultant mixture was allowed to stand at ambient temperature for 16 hours. The mixture was poured into a stirred mixture (400 ml) of ice and water. The resultant precipitate was isolated and dried under vacuum. Analysis revealed that hydrolysis of the acetate group on the 4 position of the quinazoline was incomplete. The mixture was therefore further hydrolysed with water (150 ml) and pyridine (a few drops) at 90C for 15 minutes. The resultant mixture was cooled to ambient temperature and the solid was collected by filtration, washed with water and dried under vacuum. There was thus obtained 7-ACETOXY-6-METHOXY-3, 4-dihydroquinazolin-4-one (7.4 g); NMR Spectrum: (DMSOD6) 2.3 (s, 3H), 3.9 (s, 3H), 7.45 (s, 1IN), 7.65 (s, 1H), 8. 05 (s, 1H). A mixture of A portion (2 g) of the material so obtained, thionyl chloride (32 ml) and DMF (5 drops) was stirred and heated to reflux for 1.5 hours. The mixture was cooled to ambient temperature and the excess of thionyl chloride was evaporated. Toluene was added to the residue and evaporated. The resultant residue was diluted with methylene chloride (15 ml) and a 10% ammonia solution in methanol (80 ml) was added and the mixture was heated to 80C for 10 minutes. The mixture was cooled to ambient temperature and evaporated. Water was added to the residue and the mixture was neutralised by the addition of dilute aqueous hydrochloric acid solution. The resultant precipitate was collected by filtration and dried under vacuum at 35C for 16 hours. There was thus obtained 4-chloro- 7-hydroxy-6-methoxyquinazoline (1.65 g); NMR Spectrum: (DMSOD6) 4.0 (s, 3H), 7.25 (s, 1H), 7.4 (s, 1H), 8.8 (s, 1H). Di-tert-butyl azodicarboxylate (2.3 g) was added portionwise over a few minutes to a stirred mixture of 4-chloro-7-hydroxy-6-methoxyquinazoline (1.65 g), 3-chloropropanol (0.7 ml), triphenylphosphine (2.6 g) and methylene chloride (100 ml) and the reaction mixture was stirred at ambient temperature for 2 hours. The mixture was concentrated to a volume of about 30 ml by evaporation and the residue was purified by column chromatography on silica using increasingly polar mixtures of petroleum ether (b. p 40-60C) and ethyl acetate as eluent. There was thus obtained 4-CHLORO-7- (3-CHLOROPROPOXY)-6-METHOXYQUINAZOLINE as a white solid (2 g); NMR Spectrum: (DMSOD6) 2.3 (m, 2H), 3. 8 (m, 2H), 4.05 (s, 3H), 4.4 (m, 2H), 7.45 (s, 1H), 7.55 (s, 1H), 8.9 (s, 1H).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 627-30-5, 3-Chloropropan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/81000; (2004); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 627-30-5, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 627-30-5, name is 3-Chloropropan-1-ol. A new synthetic method of this compound is introduced below.

Example 13a) [(3-Chloropropoxy)methyl]benzene; 250 ml of dichloromethane, 85 ml (0.71 mol) of benzylbromide and 10 g (0.03 mol) of tetrabutylammonium hydrogen sulfate are added to 50 ml (0.60 mol) of 3-chloro-l-propanol. A solution of sodium hydroxide (150 g, 3.75 mol) in 150 ml of water is added to the mixture under stirring. The mixture refluxed for 22 hours. After cooling down the mixture is diluted with water (100 ml), the layers are separated and the aqueous phase is shaken with dichloromethane (lx 200 ml). The organic fractions are washed with water (lx 200 ml) and subsequently dried with anhydrous sodium sulfate. The solvent is evaporated and the residue is distilled at a reduced pressure. 98.5 g (0.53 mol) of a colourless liquid are obtained, boiling point 75-82 C (26.64 Pa).-NMR (CDC13) Patent; ZENTIVA, K.S.; VLASAKOVA, Ruzena; HAJICEK, Josef; SLAVIKOVA, Marketa; WO2012/62229; (2012); A1;,
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Application of 627-30-5, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 627-30-5, name is 3-Chloropropan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

2. Preparation of 3-Chloro-1-trimethylsilyloxy-propane Lot 8853 (461-6) A one liter, three-necked flask was fitted with a large magnetic stir bar, a reflux condenser, a teflon clad thermocouple, a 250 ml. pressure-equalizing addition funnel, and an argon inlet. This apparatus was dried in an oven overnight, assembled hot, and allowed to cool to room temperature in a stream of argon. The flask was charged with 189.08 grams (2.00 mole, 1.00 equivalent) of 3-chloro-1-propanol, and 400 ml. of cyclohexane. This formed a two-phase solution. Hexamethyldisilazane, 167.86 grams (1.04 mole, 0.52 equivalent) was then added dropwise. There was an initial exotherm, then the temperature slowly declined. The reaction flask was swept with a slight positive flow of argon, above the level of the liquid. After about one third of the feed had been added, ammonia fumes were detected exiting from the apparatus with pH paper. Total feed time was ninety five minutes. At the end of the feed, the reaction mixture was homogenous. The reaction mixture was stirred at room temperature for two hours, then an aliquot was withdrawn, and analyzed by Gas Chromatography (GC). The conversion to the desired product was 74.6%. The catalyst, trimethylsilylchloride (0.5 ml.) was then added with a pipette. A white precipitate formed immediately. The reaction mixture was heated to reflux with a heating mantle. After two and three quarter hours heating, the heat source was removed. After six and a quarter hours, an aliquot was removed, and analyzed by GC. The conversion to the desired product was 92.0%. The reaction mixture was again heated to reflux, and held at reflux for an additional five hours, then allowed to stir at room temperature overnight. In the morning, the reaction mixture was still hazy. The conversion was 98.4%. The reaction mixture was heated to reflux for an additional three hours, then allowed to cool to room temperature. The reaction mixture was clear and homogenous at this time. The conversion was 98.8%. The total time the reaction mixture was at reflux was ten and three-quarters of an hour. The reaction mixture was transferred to a dry, one liter, single-necked flask. The product was purified by distillation through a twelve inch Vigreux column. The desired product had a boiling point of 154-157 C. This afforded a clear, colorless oil, yield=298.59 grams, 90.2%.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 627-30-5, 3-Chloropropan-1-ol.

Reference:
Patent; FMC Corporation; US5403946; (1995); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 627-30-5, Adding some certain compound to certain chemical reactions, such as: 627-30-5, name is 3-Chloropropan-1-ol,molecular formula is C3H7ClO, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 627-30-5.

MTCOH (8.82 g, 55 mmol) was converted to MTCOCl using standard procedures with oxalyl chloride. In a dry 250 mL round bottom flask equipped with a stir bar, the formed intermediate was dissolved in 150 mL of dry methylene chloride. Under nitrogen flow an addition funnel was attached in which 3-chloropropanol (4.94 g, 4.36 mL, 52.25 mmol), pyridine (3.95 g, 4.04 mL, 55 mmol), and 50 mL of dry methylene chloride was charged. The flask was cooled to 0 C. using an ice bath and the top solution was added drop wise during a period of 30 minutes. The formed solution was stirred for an additional 30 minutes before the ice bath was removed and the solution was stirred for an additional 16 hours under nitrogen. The crude product MTC-PrCl was directly applied onto a silica gel column and the product was separated by eluting with 100% methylene chloride. The product fractions were removed and the solvent was evaporated, yielding the product as off-white oil, which crystallized upon standing. Yield 11 g (85%). 1H-NMR (CDCl3) delta: 4.63 (d, 2H, CH2), 4.32 (t, 2H, CH2), 4.16 (d, 2H, CH2), 3.55 (t, 2H, CH2), 2.09 (m, 2H, CH2), 1.25 (s, 3H, CH3).

According to the analysis of related databases, 627-30-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; INTERNATIONAL BUSINESS MACHINES CORPORATION; Hedrick, James L.; Lee, Ashlynn L. Z.; Ng, Victor W. L.; Yang, Yi Yan; US2014/301970; (2014); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 627-30-5, Adding some certain compound to certain chemical reactions, such as: 627-30-5, name is 3-Chloropropan-1-ol,molecular formula is C3H7ClO, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 627-30-5.

Triphenylphosphine (2.6 g, 10.1 mmol) and 3-chloropropanol (0.69 ml, 8.2 mmol) were added to a suspension of 4-chloro-7-hydroxy-6-methoxyquinazoline (1.65 g, 7. 8 mmol) in dichloromethane (100 ml) under argon. The flask was placed in a water bath at 20 C and di-tert-butyl azodicarboxylate (2.30 g, 10.1 mmol) added portion wise over a few minutes. The reaction mixture was stirred at ambient temperature for 2 hours before solvent evaporation in vacuo. Purification by flash chromatography on silica gel, eluting with ethyl acetate: petroleum ether (3: 7) yielded 4-CHLORO-7- (3-CHLOROPROPOXY)-6-METHOXYQUINAZOLINE (2.0 g, 91 % yield): H-NMR (DMSO d6) : 8.90 (s, 1H), 7.55 (s, 1H), 7.45 (s, 1H), 4.42 (m, 2H), 4.05 (s, 3H), 3.80 (m, 2H), 2.31 (m, 2H).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 627-30-5, 3-Chloropropan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/113324; (2004); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 627-30-5, name is 3-Chloropropan-1-ol, molecular formula is C3H7ClO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Recommanded Product: 627-30-5

Example 1 Preparation of 5-methyl-5-(3-chloropropyl)oxycarboxyl-1,3-dioxan-2-one, (MTCOPrCl), molecular weight 236.65 A catalytic amount (3 drops) of DMF was added to a THF solution (200 mL) of MTCOH (11.1 g, 69 mmol), followed by a solution of oxalyl chloride (7.3 mL, 87 mmol) in THF (100 mL), gently added over 20 min under N2 atmosphere. The solution was stirred for 1 hour, bubbled with N2 flow to remove volatiles, and evaporated under vacuum to give the intermediate MTCCl. A mixture of 3-chloro-1-propanol (5.4 mL, 76 mmol) and pyridine (6.2 mL, 65 mmol) in dry THF (50 mL) was added dropwise to a dry THF solution (100 mL) of the intermediate MTCCl over 30 min, while maintaining a solution temperature below 0 C. with an ice/salt bath. The reaction mixture was kept stirring for another 3 hours at room temperature before it was filtered and the filtrate evaporated. The residue was dissolved in methylene chloride and washed with 1N HCl aqueous solution, saturated NaHCO3 aqueous solution, brine and water, stirred with MgSO4 overnight, and the solvent evaporated. The crude product was passed through a silica gel column by gradient eluting of ethyl acetate and hexane (50/50 to 80/20) to provide the product as a colorless oil that slowly solidified to a white solid (9.8 g, 60%).

With the rapid development of chemical substances, we look forward to future research findings about 627-30-5.

Reference:
Patent; AGENCY FOR SCIENCE, TECHNOLOGY AND RESEARCH; INTERNATIONAL BUSINESS MACHINES CORPORATION; US2012/231060; (2012); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 627-30-5 ,Some common heterocyclic compound, 627-30-5, molecular formula is C3H7ClO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

A 500 mL three-necked flask was charged with a magnetic stirrer and a thermometer, and 5.2 g of p-toluenesulfonic acid (0.03 mol) was added thereto.94.5 g of 3-chloropropanol (1.0 mol), 200 mL of dichloromethane, and 16.2 g of 3,4-dihydropyran (1.5 mol) were stirred at room temperature 20-25 C for 1 h.After the reaction liquid was subjected to gas chromatography to detect 3-chloropropanol, 100 mL of water was added to the system.After stirring for 5 min, the phases were separated, and the organic phase was washed with 100 mL of brine, dried over anhydrousDistillation under reduced pressure, collecting 110-115 C fraction (vacuum degree 30 mbar),A colorless transparent liquid of 164.6 g, which is 2-(3-chloropropoxy)tetrahydro-2H-pyran, has a GC content of 98.2% and a yield of 91.13%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,627-30-5, its application will become more common.

Reference:
Patent; Hunan Youse Chenzhoufu Chemical Co., Ltd.; Wang Gang; Peng Zhimin; Liu Bin; Li Jun; Li Zhipeng; Su Wanli; Zhang Zhenhua; (11 pag.)CN109336740; (2019); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 627-30-5 ,Some common heterocyclic compound, 627-30-5, molecular formula is C3H7ClO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

A 500 mL three-necked flask was charged with a magnetic stirrer and a thermometer, and 5.2 g of p-toluenesulfonic acid (0.03 mol) was added thereto.94.5 g of 3-chloropropanol (1.0 mol), 200 mL of dichloromethane, and 16.2 g of 3,4-dihydropyran (1.5 mol) were stirred at room temperature 20-25 C for 1 h.After the reaction liquid was subjected to gas chromatography to detect 3-chloropropanol, 100 mL of water was added to the system.After stirring for 5 min, the phases were separated, and the organic phase was washed with 100 mL of brine, dried over anhydrousDistillation under reduced pressure, collecting 110-115 C fraction (vacuum degree 30 mbar),A colorless transparent liquid of 164.6 g, which is 2-(3-chloropropoxy)tetrahydro-2H-pyran, has a GC content of 98.2% and a yield of 91.13%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,627-30-5, its application will become more common.

Reference:
Patent; Hunan Youse Chenzhoufu Chemical Co., Ltd.; Wang Gang; Peng Zhimin; Liu Bin; Li Jun; Li Zhipeng; Su Wanli; Zhang Zhenhua; (11 pag.)CN109336740; (2019); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 627-30-5, 3-Chloropropan-1-ol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, SDS of cas: 627-30-5, blongs to alcohols-buliding-blocks compound. SDS of cas: 627-30-5

A mixture of 3-chloro-1-propanol (10 g), and sodium azide (13.7 g) in water (50 mL) was heated at 90 C. overnight. Compound 3 was obtained by ether extraction

At the same time, in my other blogs, there are other synthetic methods of this type of compound,627-30-5, 3-Chloropropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; Life Technologies Corporation; Yue, Stephen; Huang, Shih-Jung; Bradford, Jolene; US8999965; (2015); B2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 627-30-5, Adding some certain compound to certain chemical reactions, such as: 627-30-5, name is 3-Chloropropan-1-ol,molecular formula is C3H7ClO, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 627-30-5.

General procedure: A 250 mL round-bottom flask equipped with aTeflon-coated magnetic stirring bar, reflux condenser and drying tube wascharged with 3.46 g (20.0 mmol, 1.0 eq) 4-bromophenol (13). It was dissolved in 100 mLDMF and 5.54 g (40.0 mmol, 2.0 eq) K2CO3, 332 mg(2.00 mmol, 10 mol%) KI and 30.0 mmol (1.5 eq) of thedesired chloroalcohol were added, respectively. Afterwards the colorlesssuspension was heated in an oil bath to 120 C and vigorously stirred atthis temperature until reaction control viaTLC showed full conversion of the starting material (20 h to 40 h).The resulting brownish suspension was cooled to room temperature and thesolvent was carefully removed in the vacuum of an oil pump. Afterwards200 mL EtOAc were added to the brownish residue, the organic phase was washedwith H2O (2 x 100 mL), brine (1 x 100 mL), dried over MgSO4,filtered and concentrated on a rotary evaporator. Finally, the brownish, oilyresidue was purified via flash column chromatography (250 g SiO2,21.0 x 6.0 cm) and the colorless liquid dried under high vacuum

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 627-30-5, 3-Chloropropan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Leypold, Mario; Wallace, Paal W.; Kljajic, Marko; Schittmayer, Matthias; Pletz, Jakob; Illaszewicz-Trattner, Carina; Guebitz, Georg M.; Birner-Gruenberger, Ruth; Breinbauer, Rolf; Tetrahedron Letters; vol. 56; 41; (2015); p. 5619 – 5622;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts