HRID1029759

反应详情

EQUATION

反应方程式

HRID 1029759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This ester (18.6 g) was heated under reflux in ethanol (50 ml) containing 2 M aqueous sodium hydroxide (50 ml) for one hour. The solvent was evaporated. The residual mixture was diluted with ice-water (300 ml) and extracted with ether (3×20 ml). The ice-cold aqueous layer was acidified to pH 1 with 6 M hydrochloric acid and extracted with ether (3×300 ml). These extracts were dried (MgSO4) and evaporated to leave an oil which was recrystallised from petrol 60°-80° C. to give 2-(2-methylfur-5-ylthio)acetic acid, (10.1 g) m.p. 35°-36° C.; NMR (90 MHz): 2.35 (s,3H), 3.50 (s,2H), 6.00 (m,1H), 6.55 (d,1H), 11.27 (br,s).

WORKUP

后处理

  1. customThe solvent was evaporated
  2. additionThe residual mixture was diluted with ice-water (300 ml)
  3. extractionextracted with ether (3×20 ml)
  4. extractionextracted with ether (3×300 ml)
  5. dry with materialThese extracts were dried (MgSO4)
  6. customevaporated
  7. customto leave an oil which
  8. customwas recrystallised from petrol 60°-80° C.