HRID377745

反应详情

EQUATION

反应方程式

HRID 377745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3,4-difluoro-α-methylcinnamic acid (28 g; 0.141 mol), PtO2 (1 g) in MeOH (250 ml) is hydrogenated at 45 p.s.i. until the theoretical uptake is completed. The catalyst is filtered off, and the material is evaporated to one-third of its original volume. A 15% potassium hydroxide solution (10 ml) is added, and the mixture is refluxed for 30 minutes. It is poured into water and extracted with ether (2×100 ml). The aqueous layer is acidified with concentrated HCl and ice, to produce an oil which is extracted into ether. The ether solution is dried over MgSO4, and is evaporated to leave 3,4-difluoro-α-methylhydrocinnamic acid (m.p. 55-56° C.) as a clear oil which crystallizes.

WORKUP

后处理

  1. filtrationThe catalyst is filtered off
  2. customthe material is evaporated to one-third of its original volume
  3. additionA 15% potassium hydroxide solution (10 ml) is added
  4. temperaturethe mixture is refluxed for 30 minutes
  5. additionIt is poured into water
  6. extractionextracted with ether (2×100 ml)
  7. customto produce an oil which
  8. extractionis extracted into ether
  9. dry with materialThe ether solution is dried over MgSO4
  10. customis evaporated