HRID35369

反应详情

EQUATION

反应方程式

HRID 35369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1-(2-pyrimidinyl)-4-piperazinyl propanol 3 g. (0.013 mol) in 50 mol. of dimethylformamide was added 3.3 g. (0.013 mol) of diphenylmethylbromide and 2.9 g. (0.034 mol) of sodium bicarbonate. The reaction mixture was refluxed overnight, dimethylformamide was evaporated under reduced pressure, and the residue was extracted with methylene chloride (400 ml.). The methylene chloride extracts were collected, washed with water and evaporated, and the remaining residue was purified by HPLC to give 1.3 g. (26% yield) of the title compound. The free base which was converted to the (1:1) fumarate salt; m.p 166°-168° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed overnight
  2. customdimethylformamide was evaporated under reduced pressure
  3. extractionthe residue was extracted with methylene chloride (400 ml.)
  4. customThe methylene chloride extracts were collected
  5. washwashed with water
  6. customevaporated
  7. customthe remaining residue was purified by HPLC
  8. customto give 1.3 g