2-Propenoic acid, 2-methyl-, 1-ethylcyclopentyl ester (9CI, ACI)

synthetischeThe preparation of 1-ethylcyclopentyl ester is as follows:It is determined that the 14 and 6 kettles of workshop 106 are thoroughly cleaned, and dichloromethane (300kg), 1-ethylcyclopentanol (20kg, 175mol), triethylamine (50kg, 494mol), 4-dimethylaminopyridine ( 0.2kg, 1.64mol) and phenothiazine (0.4kg, 2.01mol) were added to the 14 kettle. Weigh methacryloyl chloride (27.4kg, 262mol) into the 14 kettle header tank. Use frozen brine to cool down to -5 ~ 0 . The temperature is controlled at 0±5°C, the methacryloyl chloride in the high-level tank is added dropwise to the kettle, and the feed liquid in the kettle is kept at 0-5°C for 2 hours for reaction. Start sampling and testing after 2 hours of incubation, the raw material (1-ethylcyclopentanol) is less than 2.0%Add water (100kg) to the 6 kettle, transfer the feed liquid in the 14 kettle to the 6 kettle, quench, stir for 30 minutes, and let stand for 30 minutes. The kettle liquid appeared layering phenomenon, the upper water phase was separated, the lower organic layer was washed twice with 15% aqueous sodium hydroxide solution (100kg water and 15kg liquid caustic soda), and the organic layer was separated. The organic layer was washed twice with water (100 kg), and the organic layer was separated. Add anhydrous sodium sulfate (10kg) to the organic layer, dry, filter with suction, add phenothiazine (0.2kg), control the temperature to 20-25°C, and concentrate under reduced pressure to obtain the crude product. Sampling for GC detection shows that the residual solvent is less than 1.0%. The crude oil pump vacuum distillation (oil pump, 1mmHg column, main distillate temperature 4244 , external temperature 80-85 ) obtains a total of 18.5kg, 101.5mol, and 58% content is greater than 98%.