反应详情

A solution of cis-4-hydroxy-cyclohexanecarboxylic acid (10.0 g, 69.4 mmol) and a catalytic amount of concentrated sulfuric acid in methanol (700 ml) was heated at reflux over night. After cooling to room temperature the reaction mixture was neutralized by the addition of solid sodium carbonate. The mixture was stirred for 30 min, filtered and concentrated in vacuo. The residue was triturated in ethyl acetate (150 ml). The solids were removed by filtration. The filtrate was concentrated in vacuo to give the crude product (10.3 g, 94%) as colorless oil, which was used in the following steps without further purification. MS m/e: 159 (M+H+).

1. temperatureat reflux over night
2. filtrationfiltered
3. concentrationconcentrated in vacuo
4. customThe residue was triturated in ethyl acetate (150 ml)
5. customThe solids were removed by filtration
6. concentrationThe filtrate was concentrated in vacuo