HRID450497

反应详情

EQUATION

反应方程式

HRID 450497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

9.97 ml of a solution of iodomethane and then 29.44 g of K2CO3 are added, dropwise, to a solution of 34.35 g of methyl 4,5-dibromo-3-hydroxythiophene-2-carboxylate in 150 ml of DMF and the mixture is left to stir for 18 hours at AT. After cooling, the reaction mixture is diluted in 100 ml of ethyl ether and filtered, and the filtrate is concentrated under vacuum. The reaction crude is purified by silica gel chromatography, elution being carried out with heptane and then with a heptane/EtOAc mixture (85/15; v/v). 28.70 g of the expected compound are obtained.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated under vacuum
  4. customThe reaction crude
  5. customis purified by silica gel chromatography, elution