Analyzing the synthesis route of Dimethyl 2-isobutylmalonate

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

Adding a certain compound to certain chemical reactions, such as: 39520-24-6, name is Dimethyl 2-isobutylmalonate, 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 39520-24-6, HPLC of Formula: C9H16O4

To a stirred suspension of sodium hydride (60% dispersion in mineral oil, 0.997 g, 24.9 mmol) in diethyl ether (100 mL) was added dimethyl 2- isobutylmalonate (3.13 g, 16.6 mmol) dropwise. The resulting mixture was stirred at RT for 3 h. The reaction mixture was cooled to 0 C. N-chloromethyl phthalimide (3.24 g, 16.6 mmol) was added in one portion. The reaction mixture was stirred at RT overnight followed by heating to reflux for 1 h. The reaction mixture was cooled to RT and cold 1.5 N HC1 (100 mL) was added. The organic layer was separated. The aqueous layer was extracted with diethyl ether (2 x 50 mL). The combined ether layers were dried over Na2S04, filtered and concentrated under reduced pressure to afford the title compound (5.3 g, 15.2 mmol, 92 % yield). The crude product was taken to next step without further purification. LCMS (ESI) m/e 347.9 [(M+H)+, calcd for Ci8H22N06, 348.1]; LC/MS retention time (method C): tR = 1.95 min.

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

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; DZIERBA, Carolyn Diane; BRONSON, Joanne J.; MACOR, John E.; DASGUPTA, Bireshwar; NARA, Susheel Jethanand; VRUDHULA, Vivekananda M.; PAN, Senliang; HARTZ, Richard A.; RAJAMANI, Ramkumar; (199 pag.)WO2016/22312; (2016); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Continuously updated synthesis method about Dimethyl 2-isobutylmalonate

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

Adding a certain compound to certain chemical reactions, such as: 39520-24-6, name is Dimethyl 2-isobutylmalonate, 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 39520-24-6, category: esters-buliding-blocks

Taken 500mL four-necked flask was added 18.75g isobutyl-butyl malonate, 18.01g1,2,2,6,6- pentamethyl-piperidinol, 180g xylene, fitted with a reflux condenser, a thermometer, a stirrer and nitrogen, with stirring turn, was heated to 120 deg.] C, was added after 0.5h 0.48g dioctyltin oxide (first catalyst), the reaction continued at reflux for 6h, thin layer chromatography analysis showed that only the end of a significant point, transesterification . A flask was supplemented with 20g of xylene, and adding 26.15g2,6- butylated (dimethylaminomethyl) phenol (tradename antioxidant 703), and 0.41g lithium amide (second catalyst), raising the temperature to 145 deg.] C, the reaction was refluxed for 8h, TLC analysis showed that only a clear point, substitution reaction. After the heating was stopped and cooled to room temperature, the reaction mixture was added 3.5g of acetic acid, stirred for 30min, then the reaction solution was filtered dioctyltin oxide and lithium amide, washed 3 times with 70 water, water per 250ml, taken after the liquid separation the organic layer was recovered and the xylene distilled to give a tan solid which was recrystallized from ethanol and the crystals were washed, and dried to give 59.94g of light yellow powder, i.e., containing both a hindered phenol and a hindered amine structure weathering anti-aging agent. Product yield was 85.7% by HPLC analysis of purity of 94.15%.

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

Reference:
Patent; South China University of Technology; Rookie chemical (Yantai) Co., Ltd.; Cai, Zhiqi; Pi, Peng; Wenxiu, Fang; Lu, Yuan; (10 pag.)CN105294543; (2016); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics