Author: tianli

Adding a certain compound to certain chemical reactions, such as: 229027-89-8, 2-Bromo-4-fluorobenzyl Alcohol, 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: 229027-89-8, blongs to alcohols-buliding-blocks compound. Recommanded Product: 229027-89-8

General procedure: To a solution of compound 7 in DCM was added compound 8 (0.12mmol) and K2CO3 (0.24mmol) The resulting mixture was refluxed at 80C for 3h before it was quenched with 5mL of brine The organic layer was collected and purified by flash column chromatography on a silica column using cyclohexane/acetone (0-50%) to get compound 9.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,229027-89-8, 2-Bromo-4-fluorobenzyl Alcohol, and friends who are interested can also refer to it.

Reference:
Article; Pan, Ting; Ding, Yanchao; Wu, Liyang; Liang, Liting; He, Xin; Li, Qianwen; Bai, Chuan; Zhang, Hui; European Journal of Medicinal Chemistry; vol. 166; (2019); p. 480 – 501;,
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Electric Literature of 42514-50-1, 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 42514-50-1, name is 3-Amino-3-methylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

48.7 mL (668 mmol) thionyl chloride were slowly added dropwise at 0 C. with vigorous stirring to a solution of 53.0 g (514 mmol) 3-amino-3-methyl-butanol in 255 mL methylene chloride/dimethylformamide (50:1). After the addition had ended the reaction mixture was refluxed for 1 h at reflux temperature and then stirred for 16 h at ambient temperature. The solvent was removed and the residue was combined with 50 mL acetonitrile with stirring. The solid was filtered off and dried for 18 h at 45 C. 67.9 g (430 mmol, 84%) 3-chloro-1,1-dimethylpropylamine-hydrochloride were obtained as a colourless solid.

According to the analysis of related databases, 42514-50-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Boehringer Ingelheim International GmbH; US2005/245526; (2005); A1;,
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Electric Literature of 30379-58-9, 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 30379-58-9 as follows.

General procedure: The compounds 12 (A-G) were synthesized using a similar procedure. Monomethyl ester 7 (2.73 g, 10 mmol) was dissolved in 40 ml of CHCl3, and diluted thionyl chloride was added (1.1 ml, 15 mmol). The mixture was stirred at rt for 8 h. The volatile components were evaporated under reduced pressure, and the residue was dissolved in 20 ml of benzene and evaporated again. The residue was re-dissolved in 40 ml of CHCl3, and the resulting solution was added dropwise to the mixture of D-benzyl 2-hydroxy acetate 11(A-G) (10 mmol) and triethylamine (3.5 ml, 25 mmol) in 20 ml of CHCl3 at C. The solution was stirred at rt for 3 days (monitored with TLC: Petroleum ether/ethyl acetate, 2:1) and then washed successively with 1M NaOH, water, 5% HCl, water, 10% NaHCO3, and brine (25 ml of each). The organic phase was dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure to offer crude products, which were was purified by flash column chromatography eluted with petroleum ether/ethyl acetate solution to afford the compounds 12 (A-G) as colorless or light yellow viscous liquid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,30379-58-9, its application will become more common.

Reference:
Article; Jia, Chao; Yang, Ke-Wu; Liu, Cheng-Cheng; Feng, Lei; Xiao, Jian-Min; Zhou, Li-Sheng; Zhang, Yi-Lin; Bioorganic and Medicinal Chemistry Letters; vol. 22; 1; (2012); p. 482 – 484;,
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Related Products of 627-18-9, 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. 627-18-9, name is 3-Bromopropan-1-ol, molecular formula is C3H7BrO, 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.

At room temperature,In a 500 mL round bottom flask was added dichloromethane (200 mL) and p-toluenesulfonic acid (1.72 g,10 mmol), stirred and dissolved.Then 3-bromo-1-propanol (13.90 g, 100 mmol) and 2,3-dihydropyran (12.60 g, 150 mmol) were added sequentially, and the reaction was stirred for 12 h.After the reaction was completed, it was quenched with water and the organic phase was separated.The aqueous phase was extracted with dichloromethane (3×100 mL). The organic phase was washed with aq. aq.Finally purified by silica gel column chromatography (petroleum ether / ethyl acetate 30:1).Obtained yellow-green oily liquid 1-tetrahydropyranyloxy-3-bromopropane 2(19.68 g, yield 88%).

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 627-18-9, 3-Bromopropan-1-ol.

Reference:
Patent; China Agricultural University; Zhong Jiangchun; Sun Xiao; Bian Qinghua; Wang Min; Zhou Yun; Yuan Gucheng; (7 pag.)CN109970534; (2019); A;,
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Adding a certain compound to certain chemical reactions, such as: 5299-60-5, Ethyl 6-hydroxyhexanoate, 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, 5299-60-5, blongs to alcohols-buliding-blocks compound. Computed Properties of C8H16O3

PREPARATION 280 To a solution of pyridinium chlorochromate (2.0 g) in dichloromethane (15 ml) was added a solution of 6-hydroxyhexanoic acid ethyl ester (1.0 g) in dichloromethane (1.5 ml) in one portion and stirred for 1.5 hours at ambient temperature. Ether (15 ml) was added to the reaction mixture, and the insoluble material removed by filtration and discarded. The filtrate was purified by silica gel chromatography (diethyl ether) to give 6-oxohexanoic acid ethyl ester (884.6 mg), as a pale green oil. IR (KBr): 2981.4, 2940.9, 2871.5, 2827.1, 2723.0, 1731.8, 1184.1 cm-1. NMR (CDCl3, delta): 1.26 (3H, t, J=7.1 Hz), 1.5-1.8 (4H, m), 2.2-2.6 (4H, m), 4.13 (2H, q, J=7.1 Hz), 9.77 (1H, t, J=1.6 Hz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,5299-60-5, its application will become more common.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US6884868; (2005); B1;,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 7250-55-7, name is Dimethyl 3-hydroxypentanedioate, the common compound, a new synthetic route is introduced below. Product Details of 7250-55-7

Preparation 29: (l-methyl-5-oxo-pyrtOlidin-3-yl)-acetic acidStep A: 3-methanesulfonyloxy-pentanedioic acid dimethyl esterCommercially available methyl 3-hydroxy-pentanedioic acid dimethyl ester (3.5 g, 20 mmol) was dissolved in DCM (50 mL) and Et3N (5.6 mL, 40 mmol) was added thereto. The reaction solution was cooled to 0C, and MsCl (2.75 g, 24 mmol) was added dropwise thereto, followed by stirring at room temperature for 2 hours. After the reaction was complete, NH4Cl was added to the reaction solution, followed by extraction with EtOAc. The organic extract was dried over MgSO4 and concentrated under reduced pressure. The residue was purified by column chromatography (eluent: EtOAc: n-Hex = 1/5) to afford the title compound (4.77 g, 94%).MS[M+1] = 241 (M+l)

The synthetic route of 7250-55-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LG LIFE SCIENCES, LTD.; WO2009/38412; (2009); A2;,
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Related Products of 346-06-5, 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. 346-06-5, name is (2-(Trifluoromethyl)phenyl)methanol. A new synthetic method of this compound is introduced below.

a) A solution of 30 ml of phosphorus tribromide in 60 ml of absolute toluene was added dropwise at 20°-30° C. to a solution of 14 g of o-trifluoromethylbenzyl alcohol in 80 ml of absolute toluene. Subsequently, the reaction mixture was stirred at room temperature for 2 hours, the toluene was distilled under reduced pressure, the residue was dissolved in methylene chloride, treated with water and the mixture was adjusted to pH 8.0 with potassium hydrogen carbonate. The aqueous phase was extracted three times with CH2 Cl2 and the organic phases were washed twice with water and once with saturated NaCl solution, dried over Na2 SO4 and evaporated under reduced pressure. o-Trifluoromethylbenzyl bromide was obtained as the residue.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,346-06-5, (2-(Trifluoromethyl)phenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; Hoffmann-La Roche Inc.; US5270313; (1993); A;,
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Synthetic Route of 50595-15-8, 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. 50595-15-8, name is tert-Butyl 2-hydroxyacetate, molecular formula is C6H12O3, 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.

General procedure: The title compound was prepared according to the General procedure A using tert-butyl glycolate and intermediate A as starting materials. The crude product was purified by FCC (0 to 100 percent DCM in hexane). Y = 65 percent. MS ES+ ([M+Na]+): 354.4. NMR (400 MHz, DMSO-d6) delta 9.13 (s, 1H), 6.95 (s, 1H), 4.48 (s, 2H), 2.81 (t, J= 7 Hz, 4H), 2.72 (t, J= 7 Hz, 4H), 2.03 – 1.91 (m, 4H), 1.43 (s, 9H). The a-hydroxy ester or a-hydroxy acid (1 eq.) was dissolved in ACN (2 ml/mmol of a- hydroxy ester or a-hydroxy acid) and the solution was cooled down to 0° C. TEA (1 eq.) was added followed by dropwise addition of the isocyanate (1.2 eq.). The reaction mixture was allowed to warm up to room temperature and stirring was continued for 15 h under Ar. The reaction mixture was diluted with DCM and the solution was washed with 1M HCl. The aqueous layer was extracted twice with DCM and the combined organic layers were dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crude product was purified by FCC (DCM or EtOAc gradient in hexane) or by preparative reverse-phase HPLC (ACN water, 0.1 percent formic acid buffer).

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 50595-15-8, tert-Butyl 2-hydroxyacetate.

Reference:
Patent; NODTHERA LIMITED; BOCK, Mark G.; WATT, Alan Paul; PORTER, Roderick Alan; HARRISON, David; (229 pag.)WO2019/25467; (2019); A1;,
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Application of 504-63-2, 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. 504-63-2, name is 1,3-Propanediol, molecular formula is C3H8O2, 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.

(1) Put 440kg of 1,3-propanediol, 600kg of hydrochloric acid, and 3kg of benzenesulfonic acid into a 2000L glass-lined kettle with a stirring and reflux condensing device, heat up to 90 C with stirring, and keep the reaction warm;(2) After holding for 3 hours, lower the temperature of the kettle to 50 C, then put 460kg of hydrochloric acid into the kettle, continue to warm to 90 C and keep the reaction for 10 hours. The temperature of the kettle is sampled for GC analysis. When the content reaches 80%, the feed liquid is poured into the distillation kettle, and 150 kg of toluene is poured into the distillation kettle to carry out the reaction of heating and refluxing with water;(3) After the reaction with water is completed, the temperature of the kettle is reduced to room temperature, and sodium bicarbonate is added to neutralize the oil phase in the kettle to neutrality, and the salt formed by the neutralization and excess sodium bicarbonate are filtered;(4) The filtered oil phase is pumped into the rectification kettle, and the solvent toluene is concentrated under normal pressure. After the toluene is collected, the product is rectified by high vacuum. The rectified fraction is put into the reaction kettle to continue the reaction.The content detected by GC gas chromatography was 99.3%, and the product yield was 96%.

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 504-63-2, 1,3-Propanediol.

Reference:
Patent; Zouping Mingxing Chemical Co., Ltd.; Chen Qiang; Zhang Peng; Zhang Junling; Cao Xinming; Sun Fantong; Wang Tao; Du Xiaoyang; (6 pag.)CN110668918; (2020); A;,
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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.37585-25-4, name is (2-Amino-5-chlorophenyl)methanol, molecular formula is C7H8ClNO, molecular weight is 157.6, as common compound, the synthetic route is as follows.Recommanded Product: (2-Amino-5-chlorophenyl)methanol

General procedure: To a solution of 1a (1.2 g, 7.61 mmol) in CH2Cl2 (20 mL) was added MnO2 (2.6 g, 30.1 mmol) and stirred at rt under an Ar atmosphere. After 23 h with stirring, the reaction mixture was filtrated and evaporated. The residue was crystallized from AcOEt to give 7a (1.0 g, 85%) as a yellow needle crystal.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,37585-25-4, (2-Amino-5-chlorophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Ida, Yoshihiro; Matsubara, Ayaka; Nemoto, Toru; Saito, Manabu; Hirayama, Shigeto; Fujii, Hideaki; Nagase, Hiroshi; Bioorganic and Medicinal Chemistry; vol. 20; 19; (2012); p. 5810 – 5831;,
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