HRID1171442

反应详情

EQUATION

反应方程式

HRID 1171442 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of dimethyl sulfoxide (3 ml, 41.4 mmol) in dichloromethane is added to a solution of oxalyl chloride (20.7 mmol, 1.8 ml) in dichloromethane (55 ml). A solution of (2-heptyloxy-4-iodophenyl)methanol (6.55 g, 18.8 mmol) in 25 ml of dichloromethane is added dropwise to the solution previously obtained, at −78° C. The mixture is stirred until the temperature returns to room temperature. The organic phase is acidified with a 2N hydrochloric acid solution. The desired product is extracted by addition of ethyl acetate. The organic phase is washed with water, dried with magnesium sulfate and concentrated using a rotary evaporator. 6.5 g (100%) of the expected compound are recovered in the form of a yellow solid.

WORKUP

后处理

  1. custompreviously obtained, at −78° C
  2. extractionThe desired product is extracted by addition of ethyl acetate
  3. washThe organic phase is washed with water
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated
  6. customa rotary evaporator
  7. custom6.5 g (100%) of the expected compound are recovered in the form of a yellow solid