These common heterocyclic compound, 57625-74-8, name is Methyl 2-methyl-2-phenylpropanoate, 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-methyl-2-phenylpropanoate
These common heterocyclic compound, 57625-74-8, name is Methyl 2-methyl-2-phenylpropanoate, 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-methyl-2-phenylpropanoate
(b) Reaction of Methyl-alpha,alpha-dimethylphenyl acetic acid with 4-Chlorobutyryl chlorideMethyl-alpha,alpha-dimethylphenylacetic acid on Fridel-Craft’s acylation with 4-chlorobutyryl chloride in presence of anhydrous aluminum chloride in ethylene dichloride produced acylated Methyl-alpha,alpha-dimethylphenyl acetic acid, i.e., ketone intermediate as meta and para- isomers.More particularly, aluminum chloride was taken in dichloroethane and cooled in between about 0 to 2O0C. To the above pre cooled solution, Methyl-alpha,alpha-dimethylphenyl acetic acid was added at low temperature. To the reaction mixture, 4-chlorobutyryl chloride was added between about 0 to 20C. After addition of acid chloride the reaction mixture was stirred for about 8 to 10 hours at the same temperature. After completion of the reaction, mixture was quenched over chilled mixture of potable water and cone, hydrochloric acid followed by stirring the reaction mixture for another 4 hours. The reaction mixture was washed with aqueous solution of sodium bicarbonate and finally with water. Removal of dichloromethane provided Methyl-4-(4-chloro-l-oxobutyryl)-alpha,alpha-dimethylphenyl acetate (Ketone) in about 95 % HPLC purity.EXAMPLE 2Methyl-4-(4-chloro-l-oxobutyryl)- a, a-dimethyl phenyl acetate (Ketone)95 Kg (0.7124 Kmole) of aluminium chloride was taken in 120 Ltr dichloroethane and reaction mixture was cooled to 0 to 2O0C. To it was added ester of example 1, 46 Kg (0.2584 Kmole) through addition flask, maintaining the temperature 0 to 200C. Finally, to the reaction mixture was added 80 Kg (0.5673 Kmoles) of 4-chlorobutyryl chloride through addition flask maintaining the temperature 0 to 200C. After addition of acid chloride stirred the reaction mixture at 0 to 200C for 8 to 10 hours. After completion it was quenched over chilled mixture of potable water and concentrated hydrochloric acid. Then stirred the reaction mixture at 0 to 200C for 4 hours and finally extracted in dichloroethane. It was washed with 10% w/v aqueous solution of sodium bicarbonate and finally with water. Removal of the solvent under vacuum provides thick oily mass of Methyl-4-(4-chloro-l-oxobutyryl)-alpha-alpha-dimethyl phenyl acetate (Ketone). HPLC purity = 95%. Yield = 65 to 70 Kg.
The synthetic route of Methyl 2-methyl-2-phenylpropanoate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; WOCKHARDT LIMITED; JAWEED MUKARRAM, Siddiqui, Mohammed; MERWADE, Aravind, Yekanathsa; KHAN, Anjum, Reyaz; SOLANKI, Pawan, Vrajlal; WO2007/7347; (2007); A1;,
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