Month: June 2021

Application of 478375-40-5, 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 478375-40-5 as follows.

AIBN (2,2′ -azobis(2-methylpropionitrile)) (1.79 g) was added to methyl 3-bromo-5-methylbenzoate (50 g) and N-bromosuccinimide (44.7 g) in 350 mL acetonitrile, and the mixture was35 refluxed overnight. An additional11 g of N-bromosuccinimide and 0.5 g of AIBN (2,2′ -azobis(2-methylpropionitrile)) was added, and the refluxing was continued for 3 hours. The mixture was concentrated, and then taken up in 500 mL ether, and stirred for 30 minutes. The mixture was thenfiltered, and the resulting solution was concentrated. The crude product was chromatographed onsilica gel using 10% ethyl acetate in heptane to give the title compound

According to the analysis of related databases, 478375-40-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ABBVIE INC.; BOGHAERT, Erwin, R.; JUDD, Andrew, S.; PHILLIPS, Andrew, C.; SOUERS, Andrew, J.; BRUNCKO, Milan; (503 pag.)WO2017/214301; (2017); A1;,
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Adding a certain compound to certain chemical reactions, such as: 344-14-9, name is Dimethyl 2-fluoromalonate, belongs to esters-buliding-blocks compound, 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 344-14-9, HPLC of Formula: C5H7FO4

General procedure: The solution of 25% NaOMe in methanol (10.28 g, 190.38 mmol) was diluted with methanol(50 ml) under N2 atm and cooled to 0 0C. To this, compound 1a (14.90 g, 95.19 mmol) followedby compound 6 (10 g, 105.77 mmol) were added and stirred the reaction mixture at roomtemperature for 16 h. The progress of the reaction was monitored by TLC (10% Ethyl acetatein petroleum ether) showed completion of the reaction. After completion of the reaction; thereaction mixture was evaporated and solid was dissolved in H2O and acidified with Conc.HCl(~ pH 2), to give the white solid. The resulting solid was filtered and washed with water anddried under vacuum give the pure compound 7a (10 g; 48.78 mmol, 72%) as an off white solid.

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, Dimethyl 2-fluoromalonate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Sambaiah; Mallesham, Poosa; Shiva Kumar; Bobde, Yamini; Hota, Prasanta Kumar; Yennam, Satyanarayana; Ghosh, Balaram; Behera, Manoranjan; Synlett; vol. 30; 5; (2019); p. 586 – 592;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 924-99-2, name is Ethyl 3-(dimethylamino)acrylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: Ethyl 3-(dimethylamino)acrylate

b) Ethyl 3-(dimethylamino)-2-(2-fluoro-4-acetoxybenzoyl)-2-propenoate A stirred solution of Intermediate 12a (4.91 g) in DCM (80 mL) was treated with oxalyl chloride (3.25 mL) and dimethylformamide (2 drops). After 2 h the clear solution was evaporated and re-evaporated from DCM (2x). The acid chloride was re-dissolved in toluene (100 mL) and treated with triethylamine (5.17 mL) and ethyl 3- (dimethylamino)acrylate (4.13 g). After stirring for 2 h at 9O0C the mixture was cooled, filtered and the solution flash chromatographed (silica gel 40 to 100% EtOAc in petroleum ether [b.p. 40-600C]) to give the title compound as a white solid (4.3 g); APCI m/z 324.0 [M+H]+.

The synthetic route of 924-99-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; PLIVA-ISTRAZIVACKI INSTITUT D.O.O.; WO2006/50942; (2006); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 21597-54-6, name is Methyl 3-amino-2-naphthoate, belongs to esters-buliding-blocks compound, 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 21597-54-6, Recommanded Product: 21597-54-6

Mix 5.0g (11.8mmol)12-bromo-10,10-dimethyl-10hydro-indeno[1,2-b]triphenylene(12-bromo-10,10-dimethyl-10H-indeno[1,2-b]triphenylene), 2.6 g (13.0 mmol) methyl 3-amino-2-naphthoate(methyl 3-amino-2-naphthoate),.13g (0.59 mmol) Pd(OAc)2, 0.17 g (0.59 mmol)Tri-tert-butylphosphonium tetrafluoroborate, 3.9 g (17.7 mmol) sodium tert-butoxide,80 ml of toluene was degassed and placed under nitrogen and then heated at 110 C for 16 h.After the reaction was completed, the mixture was allowed to cool to room temperature.The organic layer was extracted with dichloromethane and water and dried over anhydrous MgSO4.The solvent was removed and purified by silica gel column chromatography.The product was obtained (3.2 g, yield: 51%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 3-amino-2-naphthoate, and friends who are interested can also refer to it.

Reference:
Patent; Jiguang Technology Co., Ltd.; Yan Fengwen; Deng Jinming; Zhuang Lijie; (80 pag.)CN107629068; (2018); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 75567-84-9, A common heterocyclic compound, 75567-84-9, name is Methyl 3-(4-bromophenyl)propanoate, molecular formula is C10H11BrO2, 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.

To a flask were added compound 50-6 (1.0 g, 3.5 mmol, the mixture of two trans isomers) , methyl 3- (4-bromophenyl) propionate (1.3 g, 5.3 mmol) , palladium acetate (100 mg, 0.445 mmol) , t-BuXPhos (300 mg, 0.63 mmol) , cesium carbonate (2.0 g, 6.1 mmol) and 1, 4-dioxane (10 mL) , the mixture was stirred at 90 for 3 hours and concentrated. The obtained residue was purified by silica gel column chromatography (PE/EA (V/V) = 1/1) to give the title compound as a white solid (1.0 g, 64%) . MS (ESI, pos. ion) m/z: 470.2 [M+Na] +.

The synthetic route of 75567-84-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; LIU, Xinchang; REN, Qingyun; YAN, Guanghua; GOLDMANN, Siegfried; ZHANG, Yingjun; (253 pag.)WO2019/76310; (2019); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

These common heterocyclic compound, 2065-23-8, name is Methyl 2-phenoxyacetate, 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. Recommanded Product: Methyl 2-phenoxyacetate

8.3 g of compound 2 was dissolved in 100 mL of methanol/water (9:1).12 g of lithium hydroxide was added. The reaction system was heated to 50 C and stirred for 12 h.The reaction was followed by TLC. After the reaction was over, the reaction system was added to 300 mL of ice water.Then, pH = 1 was adjusted with 6 mol/L HCl, and a large amount of white solid was formed. filter,A white solid was collected and dried in vacuo to give 6.8 g of white solid. The yield was 90%.

The synthetic route of Methyl 2-phenoxyacetate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Liaocheng University; Lei Kang; Chen Ke; Wang Shiben; Hua Xuewen; Liu Yang; Xu Xiaohua; (8 pag.)CN108570028; (2018); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 121-98-2, name is Methyl 4-methoxybenzoate, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 121-98-2

General procedure: A solution of hydrazine hydrate (20.00 mmol) in 2 mL EtOH was added dropwise to the ester 2 (5.00 mmol). The mixture was refluxed for 5 h and filtered, and the corresponding acid hydrazide 3 was obtained by washing the residue with ice water.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 121-98-2.

Reference:
Article; Han, Shuang; Zhang, Fei-Fei; Xie, Xin; Chen, Jian-Zhong; European Journal of Medicinal Chemistry; vol. 74; (2014); p. 73 – 84;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 52449-43-1, name is Methyl 4-chlorophenylacetate, belongs to esters-buliding-blocks compound, 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 52449-43-1, Product Details of 52449-43-1

[00244] Methyl 2-(4-chlorophenyl)acetate (36.7 g, 199 mmol) and paraformaldehyde(6.27 g, 209 mmol) were dissolved/suspended in DMSO (400 mL) and treated with NaOMe (537 mg, 9.94 mmol). The mixture was allowed to stir at room temperature for 2 hours to completion by thin layer chromatography (“TLC”) analysis of the crude. The reaction was poured into ice-cold water (700 mL; white emulsion) and neutralized with the addition of IM HCl solution. The aqueous layer was extracted with ethyl acetate (3 X), and the organics were combined. The organic layer was washed with water (2 X), brine (1 X), separated, dried over MgSO4, filtered, and concentrated in vacuo to afford the crude product as an oil. The residue was loaded onto a large fritted filtered with silica gel and eluted with 9:1 hexanes: ethyl acetate until the starting material/olefm were collected. The plug was then eluted with 1 :1 hexanes: ethyl acetate until the pure desired product was eluted completely. The concentrated pure fractions yielded methyl 2-(4-chlorophenyl)-3-hydroxypropanoate as an oil (39.4 g, 92%).

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-chlorophenylacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ARRAY BIOPHARMA INC.; WO2009/89359; (2009); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 4630-80-2, 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. 4630-80-2 name is Methyl cyclopentanecarboxylate, This 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.

A 2.5 M solution of BuLi in hexane (2.77 mmol; 1.1 ml; 1.2 eq) is added at -10 C. to a solution of DIPA (diisopropylethylamine) (3 mmol; 1.3 eq; 420 mul) in THF (9 ml) under inert atmosphere. The mixture is stirred for 1 hour at 0 C. This LDA solution, freshly prepared, is added dropwise to a solution of cyclopentanoic acid methyl ester in 5 ml of THF at -55 C. The mixture is stirred for 1 hour at -55 C. under inert atmosphere. HMPA (hexylmethylphophoramide) (3.46 mmol; 1.5 eq; 610 mul) is added and the mixture is stirred for 10 minutes at the same temperature. A solution of 4-methoxybenzyl mercaptan disulfide (3 mmol; 1.3 eq; 920 mg) in 12 ml of THF is then added dropwise at -55 C. After returning to room temperature, the mixture is stirred overnight. The mixture is partitioned between 10 ml of saturated NH4Cl and 20 ml of AcOEt. The organic phase is washed with saturated NH4Cl (2×10 ml), saturated NaCl (2×15 ml), dried on Na2SO4 and then concentrated under reduced pressure to yield the crude product which is purified by chromatography on silica gel. (0262) C(R2R3)=Cyclopentyl: oil (Yield: 40%) (0263) HPLC: Atlantis T3, CH3CN (0.1% TFA)/H2O (0.1% TFA) Gradient 30-90% 10 min, Rt=9.68 min (0264) NMR (CDCl3, 200 MHz): 1.60-2.40 (8H, m); 3.67 (3H, s); 3.77 (2H, s); 3.80 (3H, s); 6.83 (2H, d); 7.24 (2H, d)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl cyclopentanecarboxylate, and friends who are interested can also refer to it.

Reference:
Patent; PHARMALEADS; ROQUES, Bernard Pierre; FOURNIE-ZALUSKI, Marie-Claude; PORAS, Herve; US2015/299116; (2015); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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 344-14-9 as follows. Application In Synthesis of Dimethyl 2-fluoromalonate

A mixture of 2-fluoro-4-amidinopyridine hydrochloride (1.17 g, 6.662 mmol), dimethyl fluoromalonate (1 g, 6.662 mmol), DBU (3.35 mL, 22.4 mmol) and MeOH (50 mL) was stirred at room temperature overnight. The crude reaction mixture was evaporated under reduced pressure to yield a brown oil. A 2 N HC1 solution was cautiously added and the precipitate was collected by filtration, washed with water and dried in a vacuum oven to give the title compound (0.992 g, 66% yield). LCMS: RT 2.91 min, MI 225, Method (4LCMS1).

According to the analysis of related databases, 344-14-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CANCER RESEARCH TECHNOLOGY LIMITED; CARSWELL, Emma, L.; CHARLES, Mark, David; COCHI, Anne; DUGAN, Benjamin, J.; EKWURU, Chukuemeka, Tennyson; ELUSTONDO, Fred; FOWLER, Katherine, M.; LEROUX, Frederic, Georges, Marie; MONCK, Nathaniel, J.T.; OTT, Gregory, R.; ROFFEY, Jonathan, R.; SIDHU, Gurwinder; TREMAYNE, Neil; (305 pag.)WO2018/55402; (2018); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics