HRID1746666

反应详情

EQUATION

反应方程式

HRID 1746666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A solution of cyclohexanone (10 g, 0.10 mol) in Toluene (100 ml) was treated with 2-methoxy ethylamine (8.4 g, 0.11 mol) and refluxed at 110° C. for 3 h. The reaction mass was cooled and diluted with ethanol (50 ml) and sodium borohydride (5.8 g, 0.15 mol) was added in portions at 0° C. The reaction mass was stirred at RT for 12 h and concentrated under reduced pressure. The residue was dissolved in water (100 ml), extracted with DCM (2×100ml), dried over sodium sulphate and evaporated. The crude material was purified by column chromatography by using DCM and methanol (98:2) as eluent to afford the title compound as a pale yellow liquid.

WORKUP

后处理

  1. temperatureThe reaction mass was cooled
  2. additionwas added in portions at 0° C
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue was dissolved in water (100 ml)
  5. extractionextracted with DCM (2×100ml)
  6. dry with materialdried over sodium sulphate
  7. customevaporated
  8. customThe crude material was purified by column chromatography