Pyridine → HCID 54060299, compound

Participants

Reaction Conditions

Reaction Steps

197.8 parts of pyridine are introduced in the course of 20 minutes at -10° C., whilst stirring, into a solution of 196.3 parts of acetyl chloride in 1,350 parts of methylene chloride. 359 parts of ethylsulfamic acid chloride are then added at the same temperature. The reaction mixture is stirred for half an hour at 0° C. and one hour at 22° C. Thereafter, the mixture is stirred for 5 minutes with 800 parts of water at 9° C. and pH 1. The organic phase is then separated off from the 2-phase mixture formed, and is filtered and subjected to fractional distillation. 367 parts (79% of theory) of N-acetyl-N-ethylsulfamic acid chloride, of boiling point 34°-40° C./0.11 mbar and nD25 =1.4595, are obtained.

Provenance & Evidence