HRID932035

反应详情

EQUATION

反应方程式

HRID 932035 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 2.1 g (4.77 mmol) of N-((1S,2R)-2-(3-chlorophenyl)-1-(4-chlorophenyl)but-3-enyl)-N-(dicyclopropylmethyl)acrylamide (Example 115, Step G) in 50 mL of DCE was added 160 mg of 1,3-bis-(2,4,6-trimethylphenyl)-2-(imidazolidinylidene)(dichlorophenylmethylene)(tricyclohexylphosphine)ruthenium (“Grubb's 2nd Generation Catalyst”). The resulting mixture was degassed two times and then heated to 70° C. for 18 h. Another 160 mg of Grubb's 2nd Generation Catalyst was added at that time and heating was continued for another 18 h. The reaction mixture was cooled to room temperature. The solvent was removed and the residue was purified by chromatography on silica gel (eluent: hexane/ethyl acetate, 90/10 to 20/80) to give the title compound.

WORKUP

后处理

  1. customThe resulting mixture was degassed two times
  2. additionAnother 160 mg of Grubb's 2nd Generation Catalyst was added at that time
  3. temperatureheating
  4. temperatureThe reaction mixture was cooled to room temperature
  5. customThe solvent was removed
  6. customthe residue was purified by chromatography on silica gel (eluent: hexane/ethyl acetate, 90/10 to 20/80)