HRID1602385

反应详情

EQUATION

反应方程式

HRID 1602385 的结构方程式

PROCEDURE

实验过程

Trimethylphosphonoacetate (363 mg) in dry DME (1 ml) was added dropwise to a suspension of sodium hydride (60%; 329 mg) in dry DME (20 ml) at 0° under nitrogen. The resulting white precipitate was stirred for 40 mins at room temperature, then a solution of 7-chloro-benzofuran-4-carbaldehyde (intermediate 2) (1.238 g) in dry DME (15 ml) was added at room temperature over 1 min. The mixture was heated under reflux for 2 h, cooled to room temperature, then partitioned between water (150 ml) and ether (100 ml). The. combined organic extracts were washed with brine (100 ml) and dried (MgSO4). The solvent was evaporated to give the title compound as a colourless solid (1.59 g)

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 h
  3. temperaturecooled to room temperature
  4. custompartitioned between water (150 ml) and ether (100 ml)
  5. washcombined organic extracts were washed with brine (100 ml)
  6. dry with materialdried (MgSO4)
  7. customThe solvent was evaporated