HRID496101

反应详情

EQUATION

反应方程式

HRID 496101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

5-Acetyl-2-aminobenzenesulfonamide (see compound 13) (0.95 g, 4.4 mmol) was suspended in 96% o EtOH (50 ml) and NaBH4 (0.46 g, 12 mmol) was added in one portion. The mixture was stirred at 25° C. for 4 h and filtered through Celite and the solvent was removed under reduced pressure. The residue was treated with sat. NaHCO3 (50 ml) and extracted with EtOAc (2×50 ml), dried (Na2SO4) and evaporated to dryness. Flash-chromatography with EtOAc:n-hexane:Et3N (200:100:4, v/v/v) as eluent gave 0.35 g (37%) of 2-amino-5-(1-hydroxyethyl)benzenesulfonamide as light-brown powder. M.p. 160-162° C.

WORKUP

后处理

  1. additionwas added in one portion
  2. filtrationfiltered through Celite
  3. customthe solvent was removed under reduced pressure
  4. additionThe residue was treated with sat. NaHCO3 (50 ml)
  5. extractionextracted with EtOAc (2×50 ml)
  6. dry with materialdried (Na2SO4)
  7. customevaporated to dryness