反应详情

A solution of 26 g of 2,3-dihydro-2,2-dimethyl-7-benzofuransulfonyl chloride prepared in Example 1, in 130 ml of tetrahydrofuran, was cooled in an ice-water bath while about 30 ml of concentrated aqueous ammonium hydroxide was added portionwise at 10° to 30° C. The resulting suspension was stirred at room temperature for 3 hours, then the solvent was evaporated under reduced pressure. The residue was stirred in 150 ml of water for 0.5 hour, then filtered. The crude, wet solid was dissolved in chloroform and dried over sodium sulfate. The solvent was evaporated under reduced pressure to give a dry solid. The solid was washed once with about 100 ml of hot toluene to give 20 g of 2,3-dihydro-2,2-dimethyl-7-benzofuransulfonamide, m.p. 163°-165° C.

1. additionwas added portionwise at 10° to 30° C
2. customthe solvent was evaporated under reduced pressure
3. stirringThe residue was stirred in 150 ml of water for 0.5 hour
4. filtrationfiltered
5. dissolutionThe crude, wet solid was dissolved in chloroform
6. dry with materialdried over sodium sulfate
7. customThe solvent was evaporated under reduced pressure
8. customto give a dry solid
9. washThe solid was washed once with about 100 ml of hot toluene