反应详情

温度

0 °C

4-Phenylcyclohexanone (4 g) is dissolved under argon in MeOH (25 mL), cooled to 0° C. and treated portionwise with NaBH4 (900 mg). The mixture is stirred for 12 hours while warming to room temperature. The mixture is concentrated and then treated dropwise with water (10 mL). Then concentrated hydrochloric acid (8 mL) is added dropwise. The mixture is extracted with ethylacetate and the organic phase is washed with brine and dried (Na2SO4). The solvents are evaporated and the residue is crystallized from cyclohexane to give the title compound. TLC: rf=0.52 (silicagel, dichloromethane/ethanol 19:1).

1. temperaturewhile warming to room temperature
2. concentrationThe mixture is concentrated
3. additiontreated dropwise with water (10 mL)
4. additionThen concentrated hydrochloric acid (8 mL) is added dropwise
5. extractionThe mixture is extracted with ethylacetate
6. washthe organic phase is washed with brine
7. dry with materialdried (Na2SO4)
8. customThe solvents are evaporated
9. customthe residue is crystallized from cyclohexane