HRID2408347

反应详情

EQUATION

反应方程式

HRID 2408347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

0.19 g of 2-chloro-8,8-dimethyl-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-one are suspended in 7 mL de CH3CN, 0.58 g of cesium carbonate and 0.27 g of 2-methoxyethyl methanesulfonate are added. The mixture is heated to 65° C. for 36 h. Water, ethyl acetate are added and then after decantation, the organic phase is dried with magnesium sulfate and then evaporated. The crude is purified by flash chromatography on silica gel SiO2 (CH2Cl2/MeOH, 99/1). 0.17 g (yield=50%) of 2-chloro-9-(2-methoxyethyl)-8,8-dimethyl-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-one are obtained as a brown powder including the following characteristics:

WORKUP

后处理

  1. additionare added
  2. dry with materialafter decantation, the organic phase is dried with magnesium sulfate
  3. customevaporated
  4. customThe crude is purified by flash chromatography on silica gel SiO2 (CH2Cl2/MeOH, 99/1)