反应详情

NaSCH3 was prepared by distilling 24 g (0.50 mol) of methyl mercaptan into a stirred suspension of 24 g (0.50 mol) of 50% NaH/mineral oil in 170 ml of dimethyl sulfoxide over a 2-hr period. The mixture was charged into a 400-ml tube with 27 g (0.6 mol) of CO2 and 50 g (0.50 mol) of tetrafluoroethylene and shaken at 50° for 8 hrs. The reaction mixture was poured into a cold solution of 300 ml of concentrated HCl in 1 liter of water, and the resulting mixture was extracted continuously with ether. Removal of volatiles from the extracts at 5 mm gave 94.6 g of 3-methylthiotetrafluoropropionic acid. This acid was stirred at 85° to 95° while a mixture of 125 ml (about 1.2 mol) of 30% H2O2 and 75 ml of acetic acid was added dropwise over 2 hrs. The mixture was stirred at 90° to 95° for 3 hrs more, then evacuated at full pump to remove volatiles.

1. customNaSCH3 was prepared
2. extractionthe resulting mixture was extracted continuously with ether
3. customRemoval of volatiles from the extracts at 5 mm