HRID395569

反应详情

EQUATION

反应方程式

HRID 395569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The amine (Reference Example 7, 0.103 g, 0.24 mM) in CH2Cl2 (4 ml) was treated with triethylamine (0.073 g, 0.100 ml, 0.72 mM) and 4-dimethylaminopyridine (4-DMAP) (0.003 g, 0.024 mM), followed by a suspension of cyanogen bromide (0.129 g, 1.21 mM) in CH2Cl2 (3 ml). The solution was stirred for 1 hour. The mixture was then diluted with CH2Cl2 (7 ml), washed with sat. aq. NaHCO3 (3 ml), water (3 ml), dried and evaporated to an oil which was purified by Isolute chromatography (using as eluant 6% MeOH/CH2Cl2). The resultant oil was triturated with diethyl ether to give the title product (0.071 g, 66%).

WORKUP

后处理

  1. washwashed with sat. aq. NaHCO3 (3 ml), water (3 ml)
  2. customdried
  3. customevaporated to an oil which
  4. customwas purified by Isolute chromatography (using as eluant 6% MeOH/CH2Cl2)
  5. customThe resultant oil was triturated with diethyl ether