HRID1767611

反应详情

EQUATION

反应方程式

HRID 1767611 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% 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. filtrationfiltered through Celite
  2. customthe solvent was removed under reduced pressure
  3. additionThe residue was treated with sat. NaHCO3 (50 ml)
  4. extractionextracted with EtOAc (2×50 ml)
  5. dry with materialdried (Na2SO4)
  6. customevaporated to dryness