反应详情

温度

0 °C

111 g of freshly distilled morpholinocyclopentene, 71.7 g of triethylamine and 900 ml of chloroform are added to a round flask which is fitted with a thermometer, stirrer, reflux condenser and dropping funnel and the mixture is cooled to 0° C. Under a nitrogen atmosphere there are slowly added dropwise thereto 128 g of crude 3,3,5-trimethyl-cyclohexylacetyl chloride in 200 ml of chloroform. The flask content is stirred until it has reached a temperature of 20° C. and it is then warmed at 40° C. for a further 7 hours. After 12 hours, 76.2 of concentrated hydrochloric acid in 190 ml of water are added thereto and the flask content is held at reflux temperature for 21/2 hours. Thereafter, the organic phase is separated, the aqueous phase is extracted twice with chloroform and the combined chloroform extracts are washed as follows: three times with 10% hydrochloric acid, once with water, once with bicarbonate solution and finally with sodium chloride solution until neutral. Now it is concentrated in a rotary evaporator and the crude product (212 g) is distilled in vacuo. There are obtained 90 g (yield: 58%) of 2-(3,3,5-trimethylcyclohexylacetyl)-cyclopentanone.

1. customis fitted with a thermometer, stirrer
2. temperaturereflux condenser
3. additionUnder a nitrogen atmosphere there are slowly added dropwise
4. customa temperature of 20° C. and it
5. temperatureis then warmed at 40° C. for a further 7 hours
6. temperatureat reflux temperature for 21/2 hours
7. customThereafter, the organic phase is separated
8. extractionthe aqueous phase is extracted twice with chloroform
9. washthe combined chloroform extracts are washed
10. concentrationNow it is concentrated in a rotary evaporator
11. distillationthe crude product (212 g) is distilled in vacuo