반응 #1746
ord-989f1c45e316471198b7f2d873102bdb
반응 방정식
반응 조건
후처리
- 1기타rises to about 30° C.
- 2기타a substantially homogeneous solution is formed
- 3기타to react for 15 hours at ambient temperature
- 4기타The organic phase is separated off
- 5추출the aqueous phase is extracted with methylene chloride again
- 6세척They are washed until neutral,
- 7기타dried
- 8기타evaporated in vacuo
- 9기타The yellow oil remaining is crystallised by trituration with diisopropylether
- 10기타the solid product is recrystallised from diisopropylether
- 11기타White crystals are obtained
실험 절차
A solution of 24.3 g (0.11 mol) of O-acetyl-4-phenylcyclohexanol in 1300 ml of methylene chloride is combined with 26.0 g (0.86 mol) of paraformaldehyde and 26.0 g (0.19 mol) of zinc chloride. Hydrogen chloride is introduced into this suspension, with stirring, for 2.5 hours, whilst the temperature rises to about 30° C. and a substantially homogeneous solution is formed. The mixture is then allowed to react for 15 hours at ambient temperature and the reaction mixture is then hydrolysed with stirring in about 1.5 litres of ice water. The organic phase is separated off, the aqueous phase is extracted with methylene chloride again and the two organic phases are combined. They are washed until neutral, dried and evaporated in vacuo. The yellow oil remaining is crystallised by trituration with diisopropylether and the solid product is recrystallised from diisopropylether. White crystals are obtained, melting point 87°-89° C.