HRID1646161

反应详情

EQUATION

反应方程式

HRID 1646161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Acetoxy-4-methyl-3-pentyl-tetrahydrofuran-2-one (125.33 g, 549 mmol) is placed with 2.61 g (13.7 mmol) of p-toluenesulphonic acid and held at 150° C. for 4 hours while stirring. The acetic acid which is cleaved off is distilled off over a Vigreux column. The reaction solution, cooled to room temperature, is diluted with 500 ml of ether and washed in a separating funnel with 2×200 ml of sat. NaCl solution. Drying of the ether phase over MgSO4 and concentration on a rotary evaporator as well as distillation at 100°-103° C./0.12 mbar yields 71.34 g (77.3%) of 4-methyl-3-pentyl-2(5H)furanone.

WORKUP

后处理

  1. distillationis distilled off over a Vigreux column
  2. additionis diluted with 500 ml of ether
  3. washwashed in a separating funnel with 2×200 ml of sat. NaCl solution
  4. dry with materialDrying of the ether phase over MgSO4 and concentration on a rotary evaporator as
  5. distillationwell as distillation at 100°-103° C./0.12 mbar