反应详情

温度

70 °C

To a solution of cis-4-hydroxycyclohexanecarboxylic acid (4.00 g, 27.7 mmol) in EtOH (20 mL, 300 mmol) was added sulfuric acid (0.1 mL, 2 mmol), and the solution was heated to 70° C. for 2 h. After cooling to rt, Na2CO3 solution was added slowly to bring to pH=8. The organic solvent was removed in vacuo, and the material was extracted with EtOAc and washed with water. The organic layer was concentrated in vacuo to afford the title compound as a clear oil. 1H NMR (400 MHz, DMSO-d6): δ=1.17 (t, J=7.1 Hz, 3H), 1.42-1.56 (m, 6H), 1.73-1.86 (m, 2H), 2.26-2.39 (m, 1H), 3.60-3.71 (m, 1H), 4.04 (q, J=7.1 Hz, 2H), 4.38 (d, J=3.5 Hz, 1H).

1. temperatureAfter cooling to rt
2. customThe organic solvent was removed in vacuo
3. extractionthe material was extracted with EtOAc
4. washwashed with water
5. concentrationThe organic layer was concentrated in vacuo