反应详情

温度

75 °C

4 g (20 mmol) of 2-[(4-chlorophenyl)methyl]propane-1,3-diol, 2.94 g (20 mmol) of N-(2,2-dimethoxyethyl)acetamide, 0.3 g of paratoluenesulphonic acid and 4 ml of diethyl ether saturated with hydrogen chloride are added to 150 ml of diethyl ether. The mixture is evaporated in vacuo, then 150 ml of benzene are added twice to the residue, it is heated to 70-80° C. under a slight vacuum and the solvent is evaporated. The residue is cooled, 150 ml of dichloromethane are added, and the solution is washed with a saturated solution of sodium hydrogen carbonate then with water and dried over magnesium sulphate. The residue is purified twice by chromatography on a silica gel column eluted with chloroform, and it is finally recrystallised in a 70:4 mixture of cyclohexane/ethyl acetate. 1.7 g (6 mmol) of product are obtained.

1. customThe mixture is evaporated in vacuo
2. addition150 ml of benzene are added twice to the residue, it
3. customthe solvent is evaporated
4. temperatureThe residue is cooled
5. addition150 ml of dichloromethane are added
6. washthe solution is washed with a saturated solution of sodium hydrogen carbonate
7. dry with materialwith water and dried over magnesium sulphate
8. customThe residue is purified twice by chromatography on a silica gel column
9. washeluted with chloroform, and it
10. customis finally recrystallised in a 70:4 mixture of cyclohexane/ethyl acetate