HRID2088861

反应详情

EQUATION

反应方程式

HRID 2088861 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a solution of 1.1 g (6.3 mmol) of morpholine-3-carboxamide (a synthesis of which is described in WO-2005/026 156, Hennequin L. F. A. et al.) in acetonitrile (16 ml) are successively added 1.86 g (22.2 mmol) of sodium hydrogen carbonate powder and 0.7 ml (7.0 mmol) of isopropyl iodide, and the mixture is then heated at 150° C. by microwave for 30 minutes. The reaction mixture is cooled to room temperature, diluted with dichloromethane (30 ml) and filtered through Celite. The filtrate is concentrated under reduced pressure and 1.1 g of compound are obtained in the form of a beige-coloured powder, which is used without further purification in the following step. Yield: 97%. MH+: 173.2 (tr: 0.72 min., condition 1).

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. filtrationfiltered through Celite
  3. concentrationThe filtrate is concentrated under reduced pressure and 1.1 g of compound
  4. customare obtained in the form of a beige-coloured powder, which
  5. customis used without further purification in the following step
  6. custom173.2 (tr: 0.72 min., condition 1)