HRID1110372

反应详情

EQUATION

反应方程式

HRID 1110372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6-nitrobenzothiazole-2-sulfonamide (3.0 g, 0.011 mol), 95% ethanol (290 ml), and 10% Pd on carbon (3.0 g) was hydrogenated at an initial pressure of 50 psig for 36 hours during which time the theoretical amount of hydrogen was consumed. The reduction mixture was vacuum filtered through a pad of Celite contained in a Buchner funnel and the volatiles removed under reduced pressure. The resulting product was purified by dissolving in aqueous 10% sodium carbonate (25 ml), filtering and adjusting the pH of the filtrate to 6 with glacial acetic acid. The precipitated product was collected by vacuum filtration in a Buchner funnel and dried under reduced pressure at 78° C. in an Abderhalden to give 2.2 g (82.9% yield) of 6-aminobenzothiazole-2-sulfonamide: m.p. 221°-222° C., Anal. (C7H7N3O2S2) CHN.

WORKUP

后处理

  1. customfor 36 hours
  2. customwas consumed
  3. filtrationfiltered through a pad of Celite
  4. customthe volatiles removed under reduced pressure
  5. customThe resulting product was purified
  6. dissolutionby dissolving in aqueous 10% sodium carbonate (25 ml)
  7. filtrationfiltering
  8. filtrationThe precipitated product was collected by vacuum filtration in a Buchner funnel
  9. customdried under reduced pressure at 78° C. in an Abderhalden