N-(Methyl)nonafluorobutanesulfonamide synthesis

Yield:68298-12-4 99.68%

Reaction Conditions:

with sodium chloride in water at -8 - 0; for 4 h;

Steps:

1.1; 2.1 S1.

A 3000 mL four-necked flask with electric stirrer and thermometer was immersed in a salt water bath with a brine temperature of -8 ° C. Accurately weighed 325.5 g of a 40% aqueous solution of methylamine (4.2 mol) was added, 1120 g water was added, stirred well, 131.5 g of sodium chloride was added, stirring was continued until all the sodium chloride was dissolved. When the temperature of the kettle drops to -8 to -4 °C, 634.2 g (2.1 mol) of perfluorobutanesulfonyl fluoride was added dropwise. The temperature of the kettle was maintained below 0 ° C. After the completion of addition of the perfluorobutanesulfonyl fluoride, the reaction was kept for 4 hours. After the reaction was completed, the pH of the solution was adjusted to about 6 with hydrochloric acid to form a product floating on the liquid surface. The mixture was centrifuged to obtain perfluorobutylsulfonylmethylamine, 726.6 g of wet solid, 600 g of water was added, the temperature was raised to 50 ° C, stirred for 4 hours, and the temperature was lowered to room temperature and then digested, so that the mixture was washed twice with water and then centrifuged to obtain 666.5 g of wet material. The material was dried under vacuum at 50 ° C to obtain 655.2 g (about 2.093 mol) of the finished product in a yield of 99.68%.

References:

CN109851531,2019,A Location in patent:Paragraph 0027-0029; 0032-0034