Month: June 2021

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 99548-55-7 as follows. Safety of Methyl 4-bromo-2-methylbenzoate

General procedure: A mixture of methyl 3-bromo-2-methylbenzoate (500 mg, 3.3 mmol), NBS (770.4 mg, 4.3 mmol), and di-benzoyl peroxide (BPO, 80.7 mg, 0.3 mmol) in 1,2-dichloroethane (10 mL) was heated at 80 C for 12 h. The reaction mixture was cooled to room temperature, and the precipitated solid was removed by filtration and washed with ethers (10 mL). The filtrate was concentrated in vacuo and the residue was partitioned between 2 N NaHCO3 (15 mL) and ethers (15 mL). The organic layer was separated, dried over NaSO4, filtered and concentrated to give a crude product (683.2 mg, 89.6%), which was used in the next step reaction without further purification.

According to the analysis of related databases, 99548-55-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Li, Qing; Meng, Liuwei; Zhou, Siru; Deng, Xiaoyan; Wang, Na; Ji, Yi; Peng, Yichun; Xing, Junhao; Yao, Gongmei; European Journal of Medicinal Chemistry; vol. 180; (2019); p. 509 – 523;,
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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. 455-68-5, name is Methyl 3-fluorobenzoate, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H7FO2

General procedure: Substituted benzoic acid (1.0 mmol) was dissolved in thionylchloride and refluxed for 2 h, then the solvent was removed underreduced pressure to obtain the white solid. The white solid in methanol was added concentrated sulfuric acid (1 mL) and themixture was refluxed for 4 h, the solvent was removed to obtaincrude solid. The crude solid was extracted with ethyl acetate andwater. The solvents were evaporated to afford the pure product.Finally, the pure product was dissolved in ethanol, and the hydrazinehydrate was added. The mixture was refluxed for 9 h, and thesolvent was removed

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Lian, Zhi-Min; Sun, Juan; Zhu, Hai-Liang; Journal of Molecular Structure; vol. 1117; (2016); p. 8 – 16;,
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Electric Literature of 884497-46-5, 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. 884497-46-5, name is Methyl 3-amino-5-fluorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under argon protection,To the reactor was added 1.31 g of zinc powder (20 mmol) and 0.47 g of anhydrous lithium chloride,Join anhydrous tetrahydrofuran 10mL stirring,2.5 mol% 1,2-dibromoethane was added dropwise for 10 minutes,Then a solution of 1.81 g (10 mmol)2- (2-bromoethyl) -1,3-dioxolane in 10 mL of tetrahydrofuran,After stirring at room temperature for 3 hours,4.50g of zinc bromide (20mmol) was added with stirring,Cooled to -15 ,Then a solution of 3.22 g (12 mmol)A solution of 3-fluoro-5-methoxycarbonylbenzenediazonium tetrafluoroborate in 20 mL of tetrahydrofuran,After the addition is completed,Warmed to room temperature,1.09 g (10 mmol) of Me3SiCl,0.12 g of rhodium acetate,Heated to 87 C for 4 hours,Cool to room temperature,A small amount of dilute hydrochloric acid was added dropwise to heat to 35 C,After stirring for 2 hours,The reaction solution was extracted with ethyl acetate,The organic phase was dried and concentrated under reduced pressure.Flash column chromatography (Al2O3, ethyl acetate: petroleum ether = 1: 10),2.06 g of a white solid was obtained,Yield 93.1%

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, Methyl 3-amino-5-fluorobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tsingtao Chenda Biological Technology Co., Ltd.; Chen Linghao; (8 pag.)CN106748958; (2017); A;,
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Electric Literature of 23062-51-3, 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. 23062-51-3, name is Methyl 4-bromobicyclo[2.2.2]octane-1-carboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of XVIII-2 (6 g, 24.2 mmol) in anhydrous benzene (60.15 g) was added dropwise to an ice-water cooled suspension of AlCl3 (5.95 g, 45.1 mmol) in benzene (60.15 g) under nitrogen. The resulting reaction mixture was allowed to stirred in the ice bath for 30 min and then at rt overnight. The mixture was heated to 60 C. for 4 h and then allowed to cool to rt and poured into ice and concentrated HCl. The mixture was extracted with EtOAc, washed with brine, separated, and dried over Na2SO4 to leave an orange-brown solid, which was purified by column chromatography (PE:EA=10:1) to afford XVIII-3 (2.3 g, yield: 38.6%).

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, Methyl 4-bromobicyclo[2.2.2]octane-1-carboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Buckman, Brad Owen; Nicholas, John Beamond; Emayan, Kumaraswamy; Seiwert, Scott D.; US2014/200215; (2014); A1;,
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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. 150726-89-9, name is Dimethyl 2-(2-methoxyphenoxy)malonate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 150726-89-9

d) Na (2.3 g) was dissolved in methanol (40 ml) and 2-(3-methoxy-phenyl)-acetamidine hydrochloride (10 g) and (2-methoxyphenoxy)-malonic acid dimethyl ester (12.67 g) were added in succession at room temperature. The mixture was stirred for 5 hours at room temperature, concentrated in a rotary evaporator and the crude product was added to water. The aqueous phase was washed with ethyl acetate, adjusted to pH 1 and the precipitated crystals were sucked off and dried under a high vacuum. There was thus obtained 2-(3-methoxy-benzyl)-5-(2-methoxy-phenoxy)-pyrimidine-4,6-diol as beige crystals. MS: 354 (M)

The synthetic route of 150726-89-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-La Roche Inc.; US5837708; (1998); A;,
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Application of 145576-28-9, 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 145576-28-9 as follows.

To a solution of dry dicyclohexylamine (0.777 mL, 3.90 mmol) in toluene (20 mL) in a round-bottom flask at 0 C. under Ar was added n-butyllithium (2.44 mL, 3.90 mmol) slowly. The reaction was stirred at 0 C. for 30 min. To this prepared lithium dicyclohexylamide solution was added ethyl 4-methylenecyclohexanecarboxylate (555 mg, 3.30 mmol) in toluene (1 mL) slowly over a period of 5 min. The reaction mixture was stirred at 0 C. for additional 30 min to generate the lithium enolate. In a 5 mL pear-shaped flask was placed di-p-bromobis(tri-tert-butylphosphino)dipalladium (I) (1.2 mg, 1.5 mumol) and the flask was capped with a rubber septum. Argon gas was flushed through the flask for 10 min. 1-Bromo-3-phenoxybenzene (747 mg, 3 mmol) in toluene (1 mL) was then added. The resulting solution was transferred via cannula into the round-bottom flask containing the 0 C. THF solution of the lithium enolate of the ethyl ester. Additional toluene (2×0.5 mL) was added to the pear-shaped flask, and this solution was also transferred into the round-bottom flask by cannula. The reaction mixture was allowed to warm to rt and stirred at rt for 3 days. The reaction was quenched with saturated aq. NH4Cl and diluted with EtOAc. The organic layer was washed with water and brine, dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by preparative HPLC (PHENOMENEX Axia 5mu C18 30×100 mm column; detection at 220 nm; flow rate=40 mL/min; continuous gradient from 30% B to 100% B over 10 min+2 min hold time at 100% B, where A=90:10:0.1 H2O:MeOH:TFA and B=90:10:0.1 MeOH:H2O:TFA) to afford the title compound (221 mg, 22% yield) as a colorless oil. LCMS, [M+H]+=337.1. 1H NMR (500 MHz, CDCl3) delta 7.38-7.33 (m, 2H), 7.33-7.27 (m, 1H), 7.19-7.10 (m, 3H), 7.04-6.99 (m, 2H), 6.89 (ddd, J=8.0, 2.4, 0.8 Hz, 1H), 4.68 (s, 2H), 4.17 (q, J=7.2 Hz, 2H), 2.61-2.53 (m, 2H), 2.36-2.21 (m, 4H), 1.88-1.79 (m, 2H), 1.22 (t, J=7.0 Hz, 3H).

According to the analysis of related databases, 145576-28-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Zhang, Hao; Cheng, Peter T.W.; Chen, Sean; Tao, Shiwei; Wu, Shung C.; Negash, Lidet A.; US2014/275173; (2014); A1;,
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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. 18469-52-8, name is Methyl 4-(aminomethyl)benzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C9H11NO2

General procedure: To a solution of phenethylamine (200 mg, 1.65 mmol) and Et3N (0.64 mL, 4.95 mmol) in anhydrousTHF (2.5 mL) cooled with an ice bath, a solution of CS2 (0.12 mL, 1.98 mmol) was slowly dropped in.The reaction solution was stirred at room temperature for 0.5 h, after which AcCl (0.14 mL, 1.98 mmol)was dropped in at 0 C, and after 5 min the mixture was warmed to room temperature for 15-30 min.When the starting amine was finished, as verified by checking thin layer chromatography (T.L.C.),1MHCl (aq., 2 mL) was added to quench the reaction. The solution was extracted by EtOAc three times.All organic phases were combined and washed with brine, dried over Na2SO4, and finally filtered andconcentrated under reduced pressure. The residue was purified by column chromatography on silicagel (EtOAc/petroleum = 1/1) to provide phenethyl isothiocyanate (PEITC) (253 mg, 94%).

The synthetic route of 18469-52-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Luo, Bingling; Wang, Jiankang; Li, Xiaobing; Lu, Wenhua; Yang, Jing; Hu, Yumin; Huang, Peng; Wen, Shijun; Molecules; vol. 22; 6; (2017);,
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Electric Literature of 52727-57-8,Some common heterocyclic compound, 52727-57-8, name is Methyl 2-amino-5-bromobenzoate, molecular formula is C8H8BrNO2, 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.

Intermediate 4 (6.90 g, 30 mmol, 1.0 eq.) was added sequentially to a 100 mL dry three-necked flask with a magnetic rotor and a condensing tube.2,5-Dimethylbenzeneboronic acid (3.84 g, 31.5 mmol, 1.05 equivalent),Pd(PPh3)4 (1.04g, 0.9mmol, 0.03 equivalents),K2CO3 (8.29g, 60mmol, 2.0 equivalents),Swap three times with nitrogen, was added 1,4-dioxane (30mL) and H2O (15mL) under nitrogen.The temperature of the oil bath was raised to 100 C and the reaction was stirred for 6.0 hours.After cooling to room temperature, it was extracted three times with 30 mL of ethyl acetate.Then, filtration, distillation under reduced pressure, removal of the solvent, dry-loading, separation and purification using a silica gel column chromatography column, the eluent is petroleum ether / ethyl acetate = 20:1,5.29 g of a white solid were obtained in a yield of 69%. Used directly in the next step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-amino-5-bromobenzoate, its application will become more common.

Reference:
Patent; Zhejiang University of Technology; Ruisheng Optoelectric Science And Technology (Changzhou) Co., Ltd.; Li Guijie; Huang Da; Chen Shaohai; (53 pag.)CN109678907; (2019); A;,
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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 106685-41-0 as follows. Recommanded Product: 106685-41-0

Example 11; Preparation of 6-[3-(l-adamantyl)-4methoxy phenyl]-2 naphthoic acid (Adapalene) (I): The compound (V) (9.45 g, 22mmol) was dissolved in 1,4-Dioxane (95 ml) at reflux temperature and KOH (6.3 g, 11 mmol in 30 ml water) was added in a drop wise manner for 15 min. The reaction mixture was refluxed for 2-4 hrs and then cooled when the potassium salt of adapalene is precipitated, filtered and washed with methanol (25 ml). This salt of adapalene was acidified with 2 N HCl, solid separated, filtered and dried to obtain crude adapalene. The crude was recrystallized from THF-ethyl acetate. [Yield: 5.0 g, 81 %; Purity: HPLC > 99 %]

According to the analysis of related databases, 106685-41-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; USV LIMITED; WO2007/125542; (2007); A2;,
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