Acetic Anhydride → HCID 178474503, compound

Participants

Reaction Steps

A mixture of 6.18 g (60 mmoles) of 5-aminotetrazole with 56.3 ml of acetic anhydride was stirred at 20°-25° C. overnight. The so separated white precipitate was recovered by filtration, washed with a small volume of ethyl acetate and dried to give 3.5 g of 5-acetylaminotetrazole (Yield 45.8%). Thereafter, 10 ml of N,N-dimethylformamide and 120 mg of powdery sodium hydroxide were added to 571 mg (4.5 mmoles) of 5-acetylaminotetrazole and the resulting mixture was stirred at 20°-25° C. for one hour. Then, 1.77 g (3 mmoles) of 2,3,3-triiodoallyl-p-toluenesulfonic acid ester were added thereto and stirring was continued for 5 hours. To the reaction mixture was added water, the so separated white crystal was recovered by filtration, washed with a small volume of water and dried to give 578 mg of 5-acetylamino-1-(2',3',3'-triiodoallyl)tetrazole.

Provenance & Evidence