HRID2294004

反应详情

EQUATION

反应方程式

HRID 2294004 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 27.2 g (0.14 mol) of 5-chloromethyl-2-methyl-pyrimidin-4-ylamine hydrochloride, 29.8 g (0.14 mol) of 4-(4-fluoro-phenyl)-1,2,3,6-tetrahydropyridine hydrochloride and 42 g (0.30 mol) of dry potassium carbonate in 200 ml of dimethyl-formamide was stirred at room temperature for 18 hours. The mixture was suction filtered, the filter cake was washed with dichloromethane, the filtrate was completely freed from the solvents and the residue was crystallized twice from ethyl acetate/cyclohexane. 11.6 g (28%) of 5-[4-(4-fluoro-phenyl)-3,6-dihydro-2H-pyridin-1-ylmethyl]-2-methyl-pyrimidin-4-ylamine were obtained as yellowish crystals; m.p. 176°-178°.

WORKUP

后处理

  1. filtrationfiltered
  2. washthe filter cake was washed with dichloromethane
  3. customthe residue was crystallized twice from ethyl acetate/cyclohexane