HRID1927272

反应详情

EQUATION

反应方程式

HRID 1927272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of THF (20 mL), 2-(3-bromophenyl)-1,3-dioxolane (2.7 g) and 1,2-dibromoethane (150 mg) was added magnesium (270 mg), which was heated to reflux for 10 minutes. The reaction mixture was cooled to 0° C., and a solution of 5-methyl-2-thiophencarbaldehyde (1.0 g) and THF (5 mL) was added thereto under stirring. The reaction solution was returned to room temperature and stirred for 10 minutes. Water was added to the reaction solution, which was then extracted with ethyl acetate. The solvent was evaporated from the organic layer under a reduced pressure, and the residue was purified by silica gel chromatography (heptane:ethyl acetate=2:1) to obtain the titled compound (1.1 g).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 10 minutes
  3. customwas returned to room temperature
  4. stirringstirred for 10 minutes
  5. extractionwas then extracted with ethyl acetate
  6. customThe solvent was evaporated from the organic layer under a reduced pressure
  7. customthe residue was purified by silica gel chromatography (heptane:ethyl acetate=2:1)