HCID 86749375, compound → HCID 22419891, compound

Participants

Reaction Steps

2-amino-4-fluorobenzylsulfonate (11.0 g) was added to phosphorous oxychloride (100 ml) at 50° C. and the mixture was heated under reflux for 6 hours. The reaction mixture was concentrated in vacuo and the resulting grease was poured into ice-water mixture. A sodium hydroxide solution was added to the mixture at 0° C. until the mixture was basic. Insoluble material was filtered off and washed with water. The filtrate was treated with aqueous hydrochloric acid solution (pH=2.5). The crude product was separated by filtration. Ethyl acetate was added to the precipitate and the insoluble material was filtered off. The filtrate was concentrated in vacuo, to give 1,3-dihydro-6-fluoro-2,1-benzisothiazole 2,2-dioxide (3.2 g)

Provenance & Evidence