HRID1172990

反应详情

EQUATION

反应方程式

HRID 1172990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 5-chloro-2-methylindole (1.00 g, 6.04 mmol) in acetic acid (7 ml) was added portionwise sodium cyanoborohydride (0.76 g, 12.1 mmol) and the reaction mixture was stirred at room temperature for 16 hours. The resulting solution was diluted with ethyl acetate and washed sequentially with water and with 5 N aq. sodium hydroxide solution. The organic phase was dried over sodium sulphate and concentrated in vacuo. The residue was purified by chromatography on silica gel (eluant: heptane/ethyl acetate gradient) to yield the title compound as a colourless oil (1.00 g, 100%); MS (ISP): 170.2 ([{37Cl}M+H]+), 168.3 ([{35Cl}M+H]+).

WORKUP

后处理

  1. washwashed sequentially with water and with 5 N aq. sodium hydroxide solution
  2. dry with materialThe organic phase was dried over sodium sulphate
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by chromatography on silica gel (eluant: heptane/ethyl acetate gradient)