反应详情

Sufficient ethereal hydrogen chloride is added to 4 g (25 mmol) of 4,4-diethoxybutylamine in 500 ml of benzene to precipitate all the hydrochloride. 4 g (20 mmol) of 2-(naphthalen-1-yl)propane-1,3-diol in 200 ml of benzene and 100 mg of paratoluenesulphonic acid are then added, and the mixture is evaporated to dryness in a bath at 100° C. A further 700 ml of benzene are added, the mixture is evaporated under the same conditions, and the residue is then placed in vacuo at 100 C for 4 h. It is recrystallised in diethyl ether, dried at 60° C., recrystallised twice in ethanol, treating it with vegetable charcoal during the first recrystallisation, washed with diethyl ether and dried at 80° C. 3.2 g (10.4 mmol) of product are obtained.

1. customto precipitate all the hydrochloride
2. customthe mixture is evaporated to dryness in a bath at 100° C
3. additionA further 700 ml of benzene are added
4. customthe mixture is evaporated under the same conditions
5. customIt is recrystallised in diethyl ether
6. customdried at 60° C.
7. customrecrystallised twice in ethanol
8. additiontreating it with vegetable charcoal
9. customduring the first recrystallisation
10. washwashed with diethyl ether
11. customdried at 80° C