Month: March 2021

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. 5333-42-6, name is 2-octyldodecan-1-ol, molecular formula is C20H42O, 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. category: alcohols-buliding-blocks

Example 4 Preparation of 2-octyldodecyl phenylacetate To a 3-neck 1000 ml round-bottomed flask was added 2-octyl-1-dodecanol (240.0 g, 803.88 mmol, 1.0 equiv.), phenylacetic acid (142.28 g, 1045.0 mmol, 1.30 equiv.), toluene (240 ml) and p-toluenesulfonic acid monohydrate (1.5291 g, 8.0386 mmol, 0.010 equiv.) at room temperature. The resulting mixture was heated at reflux with stirring in an oil bath at 134 C. under a nitrogen atmosphere for 9 hours. The water produced in the reaction was collected in a Dean-Stark trap. The cooled mixture was diluted with hexanes, washed with dilute aqueous Na2CO3 solution, water, brine, dried (MgSO4), filtered, and concentrated in vacuo to afford a crude product. Excess solvent was further removed by heating the crude product with stirring in an oil bath under high vacuum for 3 hours to afford a light yellow liquid (330.0 g. 98%).

With the rapid development of chemical substances, we look forward to future research findings about 5333-42-6.

Reference:
Patent; ExxonMobil Research and Engineering Company; Ng, Man Kit; Oumar-Mahamat, Halou; Cheng, Hong; Blain, David A.; Cooper, Kathleen K.; Carey, James T.; Douglass, Michael R.; Kanga, Percy R.; Patil, Abhimanyu O.; Bodige, Satish; Lewis, Kyle G.; Hagemeister, Mark P.; (40 pag.)US2017/183595; (2017); A1;,
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Application of 402-63-1, Adding some certain compound to certain chemical reactions, such as: 402-63-1, name is 1-(3-Fluorophenyl)ethanol,molecular formula is C8H9FO, 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 402-63-1.

Example 88 5-(2-Piperidino-ethyl)-2-methyl-1H-indole-3-carboxylic Acid-1-(3-fluorophenyl)-ethyl Ester The procedure for Example 65 was followed, substituting 1-(3-fluorophenyl)-ethanol for (S)-phenylethanol, and substituting piperidine for diethylamine. ESI+MS m/z 409 (M+1).

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. 402-63-1, 1-(3-Fluorophenyl)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Millennium Pharmaceuticals, Inc.; US2003/64991; (2003); A1;,
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Electric Literature of 124-68-5, 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.124-68-5, name is 2-Amino-2-methyl-1-propanol, molecular formula is C4H11NO, molecular weight is 89.1362, as common compound, the synthetic route is as follows.

To an oven dried 250 mL round bottomed flask was weighed quinaldic acid (866 mg, 5.0 mmol). A magnetic stir bar was added and the flask was put under N2 atmosphere. The flask was charged with DCM (50 mL) and cooled to 0 C. in an ice bath. The flask was charged with N-methyl morpholine (720 muL, 7.5 mmol) and isobutlychloroformate (752 muL, 5.75 mmol) via syringe addition. The reaction was allowed to stir at 0 C. for 10 min until the solution became cloudy. At which point 2-methyl-2-aminopropanol (550 uL, 5.75 mmol) was added slowly to the flask via syringe. The reaction mixture was allowed to slowly warm to room temperature. The reaction was quenched after 2 h with 1M HCl solution (30 mL) and transferred to a separatory funnel with DCM (50 mL). The layers were partitioned and the organic phase was washed with H2O (2¡Á30 mL) and brine (1¡Á40 mL). After drying over Na2SO4 and filtration, the mixture was concentrated under reduced pressure. The crude mixture was purified by flash chromatography eluting with a 1:1 mixture of EtOAc and hexanes to afford N-(1-hydroxy-2-methylpropan-2-yl)quinoline-2-carboxamide as a colorless oil in 91% yield (1.112 g, 4.55 mmol) according to the following reaction

Statistics shows that 124-68-5 is playing an increasingly important role. we look forward to future research findings about 2-Amino-2-methyl-1-propanol.

Reference:
Patent; Sigman, Matthew Scott; Michel, Brian William; US2011/54176; (2011); A1;,
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Related Products of 83647-43-2, 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.83647-43-2, name is (3-Bromo-2-methylphenyl)methanol, molecular formula is C8H9BrO, molecular weight is 201.0605, as common compound, the synthetic route is as follows.

The compound I-1C (2 g, 10 mmol) obtained in the previous step was dissolved in dioxane (30 ml).Add 2N aqueous potassium carbonate solution (10 ml),Then, phenylboric acid (1.46 g, 12 mmol) and tetrakistriphenylphosphine palladium (150 mg, 0.12 mmol) were added, and the obtained reaction solution was replaced with nitrogen three times.The reaction was carried out at 100 C for 3 hours under a nitrogen atmosphere, and TLC showed the reaction was completed.After the methanol was rotated under reduced pressure, a saturated ammonium chloride solution (250 ml) was added.The mixture was extracted with ethyl acetate (150 mL¡Á3), and then evaporated. Ethyl acetate = 10/1 (volume ratio V / V)),Compound I-1D (1.36 g, pale yellow solid) was obtained.Yield: 68.9%.

Statistics shows that 83647-43-2 is playing an increasingly important role. we look forward to future research findings about (3-Bromo-2-methylphenyl)methanol.

Reference:
Patent; Guangzhou Dankang Pharmaceutical Biological Co., Ltd.; Xu Yong; Huang Lu; Lin Dang; Hu Hai; (29 pag.)CN110092740; (2019); A;,
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Related Products of 110-73-6, Adding some certain compound to certain chemical reactions, such as: 110-73-6, name is 2-(Ethylamino)ethanol,molecular formula is C4H11NO, 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 110-73-6.

General procedure: All compounds were prepared according our previous works[12]. The general procedure: Amines (1 mmol) was dissolved in20 mL of MeOH. Equal molar NaOH aqueous solution was added to the methanol solution. Excess CS2 was slowly dropped into thereaction flask in an ice bath. The reaction was completed at roomtemperature for 8 h. The solution was then evaporated and theresidue was precipitated three times with diethyl ether and filtered and dried to give a white powder product. All sodium dithiocarbamate(A1-22) are white solid. A1-22 and equal molar Mn(CO)5Brwere dissolved in 15mL of methanol. The solution immediately became yellow and was stirred at room temperature for 3 h. Thesolution was then evaporated and the yellow residue was dissolved in Ether. The solution was placed in 2-4 C for 2 h and the supernatant was evaporated to give a yellow solid. After recrystallization three times with DCM and CYH, the final product was obtained.

According to the analysis of related databases, 110-73-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Bai, Zhongjie; Zhang, Jinlong; Zhang, Qiuping; Zhang, Taofeng; Li, Jili; Zhao, Quanyi; Wang, Zhen; He, Dian; Cheng, Jie; Zhang, Jingke; Liu, Bin; European Journal of Medicinal Chemistry; vol. 159; (2018); p. 339 – 356;,
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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 100-37-8, name is 2-(Diethylamino)ethanol. This compound has unique chemical properties. The synthetic route is as follows. COA of Formula: C6H15NO

80 g of 2-acetylsalicylic acid was dissolved in 1000 ml of chloroform. The mixture was cooled to 5 C.103 g of 1,3-dicyclohexylcarbodiimide were added to the mixture. The mixture was stirred at room temperature for 2 hours.The solid waste was filtered off and washed with chloroform (3 x 300 ml).59 g of diethylaminoethanol was added to the reaction mixture.The mixture was stirred at room temperature for 3 hours. The organic solution was evaporated.After drying, 220 g of the desired product was obtained (96%).

With the rapid development of chemical substances, we look forward to future research findings about 100-37-8.

Reference:
Patent; TECHFIELDS INCORPORATED; YU, CHONGXI; XU, LINA; (79 pag.)JP5997658; (2016); B2;,
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Application of 100442-33-9, 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.100442-33-9, name is 1-(3,3-Diphenyl-N-methylpropylamino)-2-methyl-2-propanol, molecular formula is C20H27NO, molecular weight is 297.4345, as common compound, the synthetic route is as follows.

2,N-Dimethyl-N-(3,3-diphenylpropyl)-l-amino-2-propanol (5g) and methyl acetoactate (7.5g) were dissolved in xylene (50 ml) at 25-30C followed by the addition of zinc dust (1.75g). The reaction mixture was heated at 140-145C for 7 hours. Next,25 xylene was distilled out along with simultaneous addition of xylene in order to maintain the volume of xylene in the reaction mixture. The reaction mixture was cooled at 25- 30C followed by filtration to remove the catalyst. Distillation was carried out to remove xylene under reduced pressure. The resulting residue was degassed for 1 hour to produce title compound as viscous brown oil.

Statistics shows that 100442-33-9 is playing an increasingly important role. we look forward to future research findings about 1-(3,3-Diphenyl-N-methylpropylamino)-2-methyl-2-propanol.

Reference:
Patent; ACTAVIS GROUP PTC EHF; WO2008/107797; (2008); A2;,
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Reference of 23783-42-8 ,Some common heterocyclic compound, 23783-42-8, molecular formula is C9H20O5, 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 solution of para-toluenesulfonyl chloride (22.3 g, 105 mmol) in THF (35 mL) was added dropwise to a solution of tetraethylene glycol methyl ether (20.0 g, 96 mmol) and NaOH (6.7 g, 166 mmol) in a THF/H2O mixture (135 mL/45 ml) at 0 C. After stirring for one hour at 0 C., the reaction mixture was left to return to room temperature and then it was stirred for a further 20 hours. The solution was then poured into 200 ml of brine and the volatile materials were evaporated. The resultant mixture was extracted several times with dichloromethane and the combined organic phases were washed with brine, dried over MgSO4, filtered and evaporated under reduced pressure. The oily residue was purified by silica gel chromatography with a dichloromethane/methanol mixture (98/2) as eluent. Compound 32 is obtained in the form of a pale yellow oil in 96% yield (0310) 1H NMR (300 MHz, CDCl3) delta 2.39 (s, 3H, ArCH3), 3.31 (s, 3H, OCH3), 3.64 to 3.47 (m, 14H, OCH2CH2O), 4.11 to 4.08 (m, 2H, ArSO2OCH2), 7.28 (d, J=1.5 Hz, 2H, Ar-3,5-H), 7.73 (d, J=1.5 Hz, 2H, Ar-2,6-H); 13C NMR (75 MHz, CDCl3) delta 21.78, 59.14, 68.80, 69.45, 70.66, 70.73, 70.86, 72.07, 128.10, 129.99, 133.19, 144.96.

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. 23783-42-8, 2,5,8,11-Tetraoxatridecan-13-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; UNIVERSITE DE STRASBOURG; UNIVERSITE CLAUDE BERNARD LYON 1; HOSPICES CIVILS DE LYON; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE -CNRS; FELDER-FLESCH, Delphine; BILLOTEY, Claire; PARAT, Audrey; GAROFALO, Antonio; KRYZA, David; JANIER, Marc; (138 pag.)US2016/221992; (2016); A1;,
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Reference of 558-42-9, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 558-42-9 as follows.

Example A65Preparation of intermediate 65: 1-(4-Iodo-pyrazol-1-yl)-2-methyl-propan-2-olA mixture of 4-iodopyrazole (3 g, 15.47 mmol), 1-chloro-2-methyl-2-propanol and cesium carbonate (8.06 g, 24.75 mmol) in N,N-dimethylformamide (30 ml) was stirred at 160¡ã C. for 40 min in a sealed tube, under microwave irradiation.The mixture was diluted with water and extracted with dichloromethane.The organic layer was separated, dried (Na2SO4), filtered and the solvents evaporated in vacuo.The crude product was purified by flash column chromatography (silica; ethyl acetate in heptane 20/80 to 40/60).The desired fractions were collected and concentrated in vacuo to yield intermediate 65 (3.98 g, 97percent) as a white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,558-42-9, its application will become more common.

Reference:
Patent; Pastor-Fernandez, Joaquin; Bartolome-Nebreda, Jose Manuel; Macdonald, Gregor James; Conde-Ceide, Susana; Delgado-Gonzalez, Oscar; Vanhoof, Greta Constantia Peter; Van Gool, Michiel Luc Maria; Martin-Martin, Maria Luz; Alonso-de Diego, Sergio-Alvar; Swinney, Kelly Ann; Leys, Carina; Weerts, Johan Erwin Edmond; Wuyts, Stijn; US2011/269752; (2011); A1;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 4728-12-5, name is (2,2-Dimethyl-1,3-dioxan-5-yl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Formula: C7H14O3

To a solution of compound 24 (crude material max. 94 mmol)in dry DMF (600 ml) cooled to 0 C under argon atmosphere and NaH (60percent suspension in mineral oil; 6 g, 150 mmol, 1.6 eq.) was added. Reaction flask was filled with argon again and the mixture was stirred for 20 min. to preform sodium salt of alcohol. Benzylbromide (14.6 ml, 123 mmol, 1.3 eq.) was added and reaction flask was filled with argon again. The resulting mixture was let to warmto room temperature and stirred overnight. Water (100 ml) was added and mixture was stirred for 30 min. Solvent was evaporated in vacuo and the residue was codistilled with toluene (3). Crude material was suspended in EtOAc (250 ml) and mixture of saturatedsolution of NH4Cl (20 ml) and water (180 ml) was added.Water phase was extracted with EtOAc (2 150 ml). The organic phase was collected (250 + 150 + 150 ml) and washed with water(2 200 ml), followed by brine (1 200 ml) and dried overMgSO4. The solution was filtered and evaporated in vacuo. The residue(crude compound 25, red-brown oil) was diluted in MeOH(700 ml) and water (70 ml). DOWEX (50WX8 H+, 30 g) was addedand the mixture was heated at 50 C and stirred overnight. Reactionmixture was cooled down to room temperature and filteredthrough the frit (S3), evaporated in vacuo and codistilled withtoluene (3). Crude product 26 was obtained as brown oil andused in the next reaction step without purification. Reaction wasmonitored by TLC. Small amount of crude product was purifiedby flash chromatography (silica gel; eluent CHCl3/MeOH, gradient2?15percent) to obtain an analytical sample

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, 4728-12-5, (2,2-Dimethyl-1,3-dioxan-5-yl)methanol.

Reference:
Article; ?pa?ek, Petr; Keough, Dianne T.; Chavchich, Marina; Dra?insky, Martin; Janeba, Zlatko; Naesens, Lieve; Edstein, Michael D.; Guddat, Luke W.; Hockova, Dana; Bioorganic and Medicinal Chemistry; vol. 25; 15; (2017); p. 4008 – 4030;,
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