HRID1646161
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- distillationis distilled off over a Vigreux column
- additionis diluted with 500 ml of ether
- washwashed in a separating funnel with 2×200 ml of sat. NaCl solution
- dry with materialDrying of the ether phase over MgSO4 and concentration on a rotary evaporator as
- distillationwell as distillation at 100°-103° C./0.12 mbar