Tag: M.W=0-100

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. 764-48-7, name is Ethylene Glycol Vinyl Ether, molecular formula is C4H8O2, 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. Application In Synthesis of Ethylene Glycol Vinyl Ether

A mixture of Int-172-31 (340 mg, 1.06 mmol), Int-172-23 (0.5 mL, 5.30 mmol), K2CO3 (176 mg, 1.27 mmol), DPPP (22 mg, 0.053 mmol) and Pd(OAc)2 (2.4 mg, 0.0106 mmol) in 1,4-dioxane/H2O (2 mL, 9:1 v/v) was heated at 90 oC overnight. After the mixture was cooled to room temperature, concentrated HCl (1 mL) was slowly added and the mixture was stirred at room temperature for 1h. The product was extracted with EtOAc (3X). The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The product was purified by column chromatography using hexanes/EtOAc (0 to 20% EtOAc in hexanes) as mobile phase. The product was obtained as a pale yellow solid (128 mg) in 51% yield. LCMS: (M+1) m/z = 238.

With the rapid development of chemical substances, we look forward to future research findings about 764-48-7.

Reference:
Patent; THE SCRIPPS RESEARCH INSTITUTE; BLACKTHORN THERAPEUTICS, INC.; ROBERTS, Edward; GUERRERO, Miguel A.; URBANO, Mariangela; ROSEN, Hugh; JONES, Rob; LAXAMANA, Candace Mae; ZHAO, Xianrui; TURTLE, Eric Douglas; (331 pag.)WO2018/170492; (2018); 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;,
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Adding a certain compound to certain chemical reactions, such as: 2002-24-6, 2-Aminoethanol hydrochloride, 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, Recommanded Product: 2-Aminoethanol hydrochloride, blongs to alcohols-buliding-blocks compound. Recommanded Product: 2-Aminoethanol hydrochloride

9-(2′-hydroxyethylamino)-4-methyl-1-nitroacridine 4-Methyl-1-nitro-9-phenoxyacridine (0.33 g) is dissolved in phenol (10 g), ethanolamine hydrochloride (0.2 g) is added and the mixture is heated at 80 C. for 0.5 hour. The reaction mixture is cooled to room temperature, diluted with ether, slowly poured into dry ether (200 ml) and acidified with ethereal solution of hydrogen chloride. The resulting precipitate is filtered off, washed with ether and crystallized from absolute ethanol to give 9-(2′-hydroxyethylamino)-4-methyl-1-nitroacridine monohydrochloride as orange crystals (0.27 g, 84%), m.p. 238 C. (decomp.) 1H NMR (d6 DMSO): delta2.45 (s, 3H, CH3), 3.48 (q, 2H, H-2′), 3.65 (t, 2H, H-1′), 4.3 (t, 1H, OH), 7.1 (t, 1H, H-7), 7.24 (d, 1H, J=7.8 Hz, H-2), 7.35 (d, 1H, J=7.8 Hz, H-3), 7.5 (t, 1H, H-6), 7.65 (d, 1H, J=8 Hz, H-5), 7.75 (d,1H, J=8.0 Hz, H-8).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2002-24-6, 2-Aminoethanol hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; New York Medical College; US6589961; (2003); B2;,
Alcohol – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 534-03-2, 2-Aminopropane-1,3-diol, 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, HPLC of Formula: C3H9NO2, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C3H9NO2

Compound 2. Methylated lithocholic acid (1) (1.5 g, 3.8 mmol), serinol (0.41 g, 4.6 mmol), 1-hydroxybenzotriazole monohydrate (HOBt) (0.61 g, 4.6 mmol) was dissolved in anhydrous DMF (30 mL). 1-(3-(dimethylamino)propyl)-3-ethylcarbodiimide hydrochloride (EDC.HCl) (0.87 g, 4.55 mmol) was added in small portions at 0 C. and the resulting solution left stirring at room temperature for 20 h. The solution was taken up with EtOAc (100 mL) and was washed successively with a 1 M aqueous NaHCO3 solution (100 mL), a 0.1 M aqueous HCl solution (100 mL) and brine (2×100 mL). Then the organic layer was dried with anhydrous Na2SO4 and the solvent was removed by rotary evaporation. The reaction mixture was precipitated with ether (100 mL) and the resulting solid was collected and dried in vacuo to afford amide-containing diol (2) as a white solid (1.60 g, 91%). This product was used for next reaction without further purification. 1H NMR (300 MHz, CDCl3): delta 6.86 (d, J=7.9 Hz, 1H), 3.88-3.80 (m, 4H), 3.76-3.64 (m, 2H), 3.64-3.52 (m, 2H), 3.36 (s, 3H), 3.26-3.12 (m, 1H), 2.34-2.21 (m, 1H), 2.17-2.05 (m, 1H), 1.98-1.50 (m, 9H), 1.48-0.94 (m, 16H), 0.94-0.84 (m, 6H), 0.65 (s, 3H); 13C NMR (75 MHz, CDCl3): delta 175.4, 80.7, 61.4, 56.5, 56.0, 55.4, 52.5, 49.3, 49.0, 48.7, 48.4, 42.8, 42.1, 40.4, 40.2, 35.9, 35.6, 35.2, 34.9, 32.7, 31.8, 28.2, 27.3, 26.7, 26.4, 24.2, 23.4, 20.8, 18.3, 12.0; MS (MALDI-TOF): calcd. for C28H49NO4 [M+Na]+ 486.3554, found 486.3570.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,534-03-2, 2-Aminopropane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; WISCONSIN ALUMNI RESEARCH FOUNDATION; Gellman, Samuel Helmer; Chae, Pil Seok; Kobilka, Brian; Rasmussen, Soren; US2013/266656; (2013); A1;,
Alcohol – Wikipedia,
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Application of 3279-95-6, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.3279-95-6, name is 2-(Aminooxy)ethanol, molecular formula is C2H7NO2, molecular weight is 77.08, as common compound, the synthetic route is as follows.

[0277] To a solution of the product of Example 2, Step B, 2-(2-chloro-4-iodo-phenylamino)-3,4-difluorobenzoic acid pentafluorophenyl ester (10.0 g, 17.4 mmol), in anhydrous dimethylformamide (36 mL) was added 2-(aminooxy)-ethanol [prepared by the literature procedure: Dhanak, D.; Reese, C. B., J. Chem. Soc., Perkin Trans. 1987;1:2829] (1.6 g, 20.8 mmol) and N,N-diisopropylethylamine (6.0 mL, 34.8 mmol). The resultant solution was stirred at ambient temperature for 16 hours. The reaction mixture was concentrated to 20% volume then diluted with ethyl acetate (360 mL). The resultant solution was washed with water (6×60 mL) and brine (2×60 mL). The organics were dried over anhydrous magnesium sulfate and concentrated under reduced pressure to afford a white solid that was purified on silica gel. Elution with ethyl acetate-methanol (9:1) afforded 2-(2-chloro-4-iodo-phenylamino)-3,4-difluoro-N-(2-hydroxy-ethoxy)-benzamide (7.31 g, 90%) as a white solid. Recrystallization from methanol afforded analytically pure material: m.p. 173-175 C.; 1H NMR (400 MHz, DMSO-d6) delta 11.93 (br s, 1H), 8.85 (br s, 1H), 7.76 (d, J=1.7 Hz, 1H), 7.48 (dd, J=8.6, 1.7 Hz, 1H), 7.44 (dd, J=8.5, 6.2 Hz, 1H), 7.25 (dt, J=8.5, 9.3 Hz, 1H), 6.58 (dd, J=8.5, 6.4 Hz, 1H), 4.70 (br s, 1H), 3.86 (br s, 2H), 3.56 (br d, J=3.9 Hz, 2H); MS (APCI+)=469.0; MS (APCI-)=467.0; [0278] Anal. Calcd/found for C15H12ClF2IN2O3: C, 38.45/38.60; H, 2.58/2.53; N, 5.98/5.91; F, 8.11/8.08; I, 27.08/27.43.

Statistics shows that 3279-95-6 is playing an increasingly important role. we look forward to future research findings about 2-(Aminooxy)ethanol.

Reference:
Patent; Rewcastle, Gordon William; Spicer, Julie Ann; Barrett, Stephen Douglas; Kaufman, Michael David; Milbank, Jared Bruce John; Tecle, Haile; US2004/6245; (2004); A1;,
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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. 109-83-1, name is 2-(Methylamino)ethanol. A new synthetic method of this compound is introduced below., Product Details of 109-83-1

A solution of 4-methoxy-2,3,6-trimethylbenzenesulfonyl chloride (2.29 g, 9.19 mmole) in THF (30 ml) was added dropwise at 0 C. to a solution of 2-methylaminoethanol (0.95 ml, 11.8 mmole) and triethylamine (5 ml) in THF (15 ml). The mixture was then stirred for 5 hours at RT, concentrated by evaporation in vacuo, and the residue was taken up in NaHCO3 solution and extracted with ethyl acetate (3×30 ml). The combined organic phases were dried with Na2SO4 and concentrated by evaporation in vacuo. Yield: 2.38 g, 90%.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 109-83-1, 2-(Methylamino)ethanol.

Reference:
Patent; GRUENENTHAL GmbH; US2009/186899; (2009); A1;,
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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. 156-87-6, name is 3-Aminopropan-1-ol, molecular formula is C3H9NO, 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. Computed Properties of C3H9NO

A solution of 3-aminopropan-1-ol (3 g, 39.9 mmol) and benzaldehyde (4.05 mL, 39.9 mmol) in methanol (200 mL) was stirred at room temperature overnight. The solution was cooled to 0 C., and sodium borohydride (1.813 g, 47.9 mmol) was added slowly in several portions. The resulting mixture was stirred at room temperature for three hours, and then it was partitioned between water and dichloromethane (3*). The organic extracts were combined and dried over Na2SO4, the drying agent was removed by filtration, and the solution was concentrated in vacuo to give the title compound as an oil (6.5 g, 98%)

With the rapid development of chemical substances, we look forward to future research findings about 156-87-6.

Reference:
Patent; ABBVIE INC.; Bhatia, Pramila A.; Randolph, John T.; Schrimpf, Michael R.; Zhang, Quinwei I.; US2014/171423; (2014); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 3279-95-6, 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. 3279-95-6, name is 2-(Aminooxy)ethanol, molecular formula is C2H7NO2, 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.

To a solution of 7-(4-chlorophenyl)-1-methyl-6,7-dihydro-5H-benzo[f][1,2,3]triazolo[1,5-d][1,4]diazepine-9-carboxylic acid (55.6 mg, 0.157mmol) in THF (4 mL) was added HATU (89.4 mg, 0.235 mmol) at 0 C and the reaction mixture was stirred for 30 min. Triethylamine (47.4 mg, 0.470 mmol) and 2-(aminooxy)ethanol (18.1 mg, 0.235mmol) were then added. The resulting mixture was stirred at RT overnight and partitioned between water and DCM. The organics was extracted with DCM (3 x 20 mL) and the combined organic layer were washed with brine (2 x 30 mL), dried and concentrated under reduced pressure. The crude product was purified by preparative TLC (DCM: MeOH= 10: 1) to give 7-(4-chlorophenyl)-N-(2-hydroxyethoxy)-1-methyl-6,7-dihydro- 5H-benzo[f][1,2,3]triazolo[1,5-d][1,4]diazepine-9-carboxamide (18 mg, 28%) as a yellow solid. LCMS (Method B):: RT 2.48 min m/z 414.1 [M+H]+

According to the analysis of related databases, 3279-95-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CATALYST THERAPEUTICS PTY LTD; BURNS, Chris; GARNIER, Jean-Marc; SHARP, Phillip Patrick; FEUTRILL, John; CUZZUPE, Anthony; (140 pag.)WO2017/20086; (2017); A1;,
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Related Products of 124-68-5 ,Some common heterocyclic compound, 124-68-5, molecular formula is C4H11NO, 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 (2-Hydroxy-1,1-dimethyl-ethyl)-carbamic acid tert-butyl ester 2-Amino-2-methyl-propan-1-ol (53 g, 0.59 mol) and di-tert-butyl dicarbonate (65.0 g, 0.297 mol) were combined in H2O (500 mL) and stirred at 25 C. for 1 h. The reaction mixture was extracted with CHCl3 (2*250 mL) The organics were dried and concentrated to a white amorphous solid which was recrystallized from hot hexanes to afford desired material (30 g, 53%) as a white solid: 13C NMR (CD3OD, 100 MHz) delta 157.76, 80.135, 70.095, 54.992, 29.247, 24.695.

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. 124-68-5, 2-Amino-2-methyl-1-propanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Lombardo, Louis J.; Bhide, Rajeev S.; Kim, Kyoung S.; Lu, Songfeng; US2003/232832; (2003); A1;,
Alcohol – Wikipedia,
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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