反应详情

9.6 g of aluminium, 2.8 g of aluminium isopropylate, 0.2 g of mercuric chloride and 130 g of secondary butyl alcohol are introduced into a flask and the mixture is brought to reflux. Once the aluminium has started to react, 390 g of secondary butyl alcohol are slowly added over 45 minutes, maintaining reflux. Heating is then dicontinued and the mixture is left to attain the ambient temperature, stirring is discontinued and a calcium chloride drying tube is fitted. The mixture in then left overnight. On the following day, the mixture is brought to reflux and 332 g of 1,5,5-trimethyl-4-acetyl-cyclohex-1-ene are added in the course of about 2 hours. When the vapour temperature reaches 80°, the methyl ethyl ketone formed starts to distill off; the duration of the distillation is about 6 hours--finally under a pressure of 50 mm of mercury. The residue is taken up in 500 ml of benzene and washed twice with 100 ml of 10% sulphuric acid, twice with 100 ml of water, twice with 100 ml of a sodium bicarbonate solution and then with water until neutral. Distillation of the solvent over a water bath under reduced pressure gives 322 g of crude product, which are fractionated in a 500 ml three-necked flask fitted with a 1 meter adiabatic column having an unoxidisable filling with a particle size of 4×4 mm. 190.8 g of 1,5,5-trimethyl-4-(1-hydroxyethyl)-cyclohex-1-ene (57%) are obtained, having the following physical properties:

1. temperatureto reflux
2. customto react
3. temperaturemaintaining
4. temperaturereflux
5. temperatureHeating
6. waitthe mixture is left
7. customthe ambient temperature
8. customa calcium chloride drying tube is fitted
9. temperatureto reflux
10. customreaches 80°
11. distillationthe methyl ethyl ketone formed starts to distill off
12. distillationthe duration of the distillation
13. waitis about 6 hours
14. washwashed twice with 100 ml of 10% sulphuric acid, twice with 100 ml of water, twice with 100 ml of a sodium bicarbonate solution
15. distillationDistillation of the solvent over a water bath under reduced pressure
16. customgives 322 g of crude product, which
17. customare fractionated in a 500 ml three-necked flask
18. customfitted with a 1 meter adiabatic column