HRID496101
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added in one portion
- filtrationfiltered through Celite
- customthe solvent was removed under reduced pressure
- additionThe residue was treated with sat. NaHCO3 (50 ml)
- extractionextracted with EtOAc (2×50 ml)
- dry with materialdried (Na2SO4)
- customevaporated to dryness