تفاعل #1746
ord-989f1c45e316471198b7f2d873102bdb
معادلة التفاعل
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1أخرىrises to about 30° C.
- 2أخرىa substantially homogeneous solution is formed
- 3أخرىto react for 15 hours at ambient temperature
- 4أخرىThe organic phase is separated off
- 5استخلاصthe aqueous phase is extracted with methylene chloride again
- 6غسيلThey are washed until neutral,
- 7أخرىdried
- 8أخرىevaporated in vacuo
- 9أخرىThe yellow oil remaining is crystallised by trituration with diisopropylether
- 10أخرىthe solid product is recrystallised from diisopropylether
- 11أخرىWhite crystals are obtained
الإجراء التجريبي
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.