反应详情

20.0 g of 1,5,5-trimethyl-4-(1-hydroxyethyl)-cyclohex-1-ene are introduced into a 1 liter three-necked flask provided with a mechanical stirrer, a heater, a dropping funnel and a reflux condenser fitted with a calcium chloride drying tube. 273 g of formic acid are then added in the course of 1/2 hour, whilst maintaining the temperature of the reaction mixture between 0° and 5°. After the end of the addition, the temperature of the composition is maintained at 5°. The composition is then slowly heated over 2 hours to 20°-25°. The mixture is then poured into 200 ml of water and extracted with benzene. The combined benzene extracts are washed successively with water, a solution of sodium bicarbonate and, finally, with water again. After distillation of the solvent over a water bath, the crude ester is distilled under a pressure of 0.05 mm of mercury. 11.0 g of 1,5,5-trimethyl-4-(1-formyloxyethyl)-cyclohex-1-ene are obtained, having the following physical constants:

1. customprovided with a mechanical stirrer
2. customa heater, a dropping funnel and a reflux condenser fitted with a calcium chloride drying tube
3. temperaturewhilst maintaining the temperature of the reaction mixture between 0° and 5°
4. additionAfter the end of the addition
5. temperaturethe temperature of the composition is maintained at 5°
6. temperatureThe composition is then slowly heated over 2 hours to 20°-25°
7. extractionextracted with benzene
8. washThe combined benzene extracts are washed successively with water
9. distillationAfter distillation of the solvent over a water bath
10. distillationthe crude ester is distilled under a pressure of 0.05 mm of mercury