HRID2419210

反应详情

EQUATION

反应方程式

HRID 2419210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The latter ester (25 g) is stirred in 500 ml of 5% aqueous KOH in methanol (250 ml H2O, 250 ml CH3OH, 25 g KOH) at room temperature for about 2 hr. The mixture is diluted with water and extracted several times with ether to remove all neutral material. The aqueous fraction is cooled with crushed ice, acidified with 10% HCl and extracted with ether. The ether extract is washed with water and brine, dried (MgSO4) and concentrated to give 5-methoxy-2-thiopheneglyoxylic acid (3; X1 = CH3O, X2 and X3 = H and R10 = H); γmaxCHCl3 3000, 1630, 1625, 1530 cm-1.

WORKUP

后处理

  1. extractionextracted several times with ether
  2. customto remove all neutral material
  3. temperatureThe aqueous fraction is cooled with crushed ice
  4. extractionextracted with ether
  5. extractionThe ether extract
  6. washis washed with water and brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated