HRID489712

反应详情

EQUATION

反应方程式

HRID 489712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Concentrated H2SO4 (1 ml) was added to a solution of 1,4-dihydrobenzoic acid (3 g, 23.97 mmol) in freshly dried methanol (10 ml). The reaction was heated to reflux in air for 1 h, cooled, poured into H2O (25 ml) and extracted with ether (3×50 ml). The combined ether layers were washed with 5% Na[HCO3] solution (50 ml) and saturated NaCl solution (50 ml) and dried over MgSO4. The ether was removed on the rotary evaporator to leave a colourless oil which was used without further purification.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureto reflux in air for 1 h
  3. temperaturecooled
  4. extractionextracted with ether (3×50 ml)
  5. washThe combined ether layers were washed with 5% Na[HCO3] solution (50 ml) and saturated NaCl solution (50 ml)
  6. dry with materialdried over MgSO4
  7. customThe ether was removed on the rotary evaporator
  8. customto leave a colourless oil which
  9. customwas used without further purification