HRID1913763

反应详情

EQUATION

反应方程式

HRID 1913763 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

460 mg (2 mmol) of 1-(chloromethyl)-4-(2-phenylethyl)benzene [preparation according to M. Carrara et al., Arzneim. Forsch. 47 (7), 803-809 (1997)] and 414 mg (3 mmol) of anhydrous potassium carbonate are added to a solution of 411 mg (1 mmol) of methyl 4-[(3E)-2-[2-(4-cyanophenyl)ethyl]-4-(2-hydroxyphenyl)but-3-en-1-yl]benzoate in 10 ml of dry acetonitrile, and the mixture is heated under reflux for 12 hours. The mixture is then evaporated to dryness. The residue is taken up in ethyl acetate, washed with water and with saturated sodium chloride solution and dried over sodium sulphate. After filtration, the organic phase is evaporated and the resulting crude product is purified by preparative HPLC. 431 mg (0.7 mmol, 65% yield) of a solid are obtained.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 12 hours
  3. customThe mixture is then evaporated to dryness
  4. washwashed with water and with saturated sodium chloride solution
  5. dry with materialdried over sodium sulphate
  6. filtrationAfter filtration
  7. customthe organic phase is evaporated
  8. customthe resulting crude product is purified by preparative HPLC