反应详情

温度

130 °C

A mixture of 3-(2-oxo-1-phenylcyclohexyl)propanoic acid (1 g, 4.06 mmol), potassium hydroxide (0.770 g, 13.72 mmol), hydrazine monohydrate (0.348 mL, 6.09 mmol), and ethylene glycol (5 mL) was heated to 130° C. for 1.5 h. The condenser was removed and the mixture was heated to 200° C. for 30 min. The reaction mixture was then heated under reflux with a reflux condenser for additional 1.5 h. The reaction mixture was cooled to room temperature and diluted with 1N HCl to a total reaction volume of 25 mL. The precipitated product was collected by filtration, washed several times with water, and dried in vacuo to obtain 3-(1-phenylcyclohexyl) propanoic acid as a white solid (Int. 2, 923 mg, 93% yield). HPLC: tR=3.7 min, Chromolith SpeedRod 4.6×50 mm, 4 min gradient, Detection Wave length 220 nm, Starting solvent: 10% aq. MeOH-0.2% H3PO4; Final solvent: 90% aq. MeOH-0.2% H3PO4. LC/MS: m/e 215.19 (M+H-H2O)+.

1. customThe condenser was removed
2. temperaturethe mixture was heated to 200° C. for 30 min
3. temperatureThe reaction mixture was then heated
4. temperatureunder reflux with a reflux condenser for additional 1.5 h
5. temperatureThe reaction mixture was cooled to room temperature
6. additiondiluted with 1N HCl to a total reaction volume of 25 mL
7. filtrationThe precipitated product was collected by filtration
8. washwashed several times with water
9. customdried in vacuo