HRID1965961

反应详情

EQUATION

反应方程式

HRID 1965961 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

To a solution of 1-but-3-ynyl-3-(2-chloro-ethyl)-urea (5 g, 28.7 mmol) in THF (100 mL) add tetrabutylammonium bromide (1.82 g, 5.65 mmol) and potassium hydroxide (2.01 g, 35.9 mmol). Heat the resulting suspension at 75° C. for 72 h and allow to cool to room temperature. Dilute the mixture with EtOAc (200 mL), wash with water (2×100 mL) and 1N aqueous HCl (100 mL). Dry the organic phase over MgSO4, filter and concentrate in vacuo to obtain the title compound as a white powder (816 mg, 21%).

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. washwash with water (2×100 mL) and 1N aqueous HCl (100 mL)
  3. dry with materialDry the organic phase over MgSO4
  4. filtrationfilter
  5. concentrationconcentrate in vacuo