HRID275931

反应详情

EQUATION

反应方程式

HRID 275931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

o-Toluidine(0.48 ml, 4.5 mmol) and triethylamine were added to a solution of 6-methoxymethyl-5-methyl-2-chloro-4-(1,2,3,4-tetrahydroisoquinolin-2-yl)pyrimidine (0.9 g, 3 mmol) in dimethylformamide(5 ml) and stirred for 5 hours at 130° C. The reaction mixture was cooled to a room temperature, diluted with dichloromethane, and washed with aqueous sodium hydroxide and water. The organic layer was dried over anhydrous magnesium sulfate, concentrated, and the residual oil was purified by column chromatography. The purified compound was dissolved in ethyl ether. Ethyl ether saturated with hydrochloric acid was added to a mixture solution. The resulting solid was filtered and dried to give 400 mg of the titled compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to a room temperature
  2. washwashed with aqueous sodium hydroxide and water
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customthe residual oil was purified by column chromatography
  6. dissolutionThe purified compound was dissolved in ethyl ether
  7. additionEthyl ether saturated with hydrochloric acid was added to a mixture solution
  8. filtrationThe resulting solid was filtered
  9. customdried