反应详情

97.0 g (0.597 mol) of 4-t-butylcyclohexanone and 134.7 g (1.184 mol) of 3-chloro-1,2-propanediol are dissolved in 1100 ml of toluene in the presence of 11.5 g (0.060 mol) of PTSA. The mixture is brought to reflux for 6 hours while removing the water formed using a Dean-Stark trap. The reaction mixture is brought to room temperature and washed twice with 1500 ml of an aqueous solution containing 5% of NaHCO3. The organic phase is dried over MgSO4 and concentrated under vacuum. The residual oil is used directly in the following step (yield: 99%; NMR analysis)

1. temperatureto reflux for 6 hours
2. customwhile removing the water
3. customformed
4. customis brought to room temperature
5. washwashed twice with 1500 ml of an aqueous solution
6. additioncontaining 5% of NaHCO3
7. dry with materialThe organic phase is dried over MgSO4
8. concentrationconcentrated under vacuum