反应详情

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.

1. customrises to about 30° C.
2. customa substantially homogeneous solution is formed
3. customto react for 15 hours at ambient temperature
4. customThe organic phase is separated off
5. extractionthe aqueous phase is extracted with methylene chloride again
6. washThey are washed until neutral,
7. customdried
8. customevaporated in vacuo
9. customThe yellow oil remaining is crystallised by trituration with diisopropylether
10. customthe solid product is recrystallised from diisopropylether
11. customWhite crystals are obtained