HRID553958

反应详情

EQUATION

反应方程式

HRID 553958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Grubbs catalyst 2nd generation (285 mg) was added to a solution of methyl (E)-3-[(3S,5R)-4-(3-butenoyl)-5-(3,4,5-trifluorophenyl)morpholin-3-yl]acrylate (1.24 g) in dichloromethane (100 mL), and the reaction solution was heated under reflux in a nitrogen atmosphere for 1.5 hours. The reaction solution was returned to room temperature. Triethylamine (3 mL) was added to the reaction solution, which was then stirred for 10 minutes. The reaction solution was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (heptane-ethyl acetate system) to obtain 250 mg of the title compound. The property values of the compound are as follows.

WORKUP

后处理

  1. temperaturethe reaction solution was heated
  2. temperatureunder reflux in a nitrogen atmosphere for 1.5 hours
  3. customwas returned to room temperature
  4. concentrationThe reaction solution was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (heptane-ethyl acetate system)