HRID2229138

反应详情

EQUATION

反应方程式

HRID 2229138 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(2-Fluoro-4-nitrophenyl)tetrahydro-2-(2-propenyl)-2H-1,2-thiazine 1,1-dioxide (1.303 g, 4.15 mmol) and cuprous bromide: dimethyl sulfide complex (0.855 g, 4.15 mmol) are stirred at ice temperature in dry THF (30 ml). Sodium borohydride (1.25 g, 33.07 mmol) is added and the mixture stirred for 20 min. Methanol (10 ml) is carefully added over 30 min followed by ammonium chloride solution (50 ml). The mixture is extracted with methylene chloride (2×100 ml), washed with water (50 ml) and brine (50 ml), dried (MgSO4) and evaporated to yield the product as a cream solid (1.178 g, 100%) mp 96°.

WORKUP

后处理

  1. extractionThe mixture is extracted with methylene chloride (2×100 ml)
  2. washwashed with water (50 ml) and brine (50 ml)
  3. dry with materialdried (MgSO4)
  4. customevaporated