反应详情

A solution of 3-ethylhexahydro-3-(3-hydroxyphenyl)-1-methyl-2H-azepin-2-one (1.5 g) in dry tetrahydrofuran was added to a stirred suspension of aluminium lithium hydride (0.48 g) and heated under reflux for 5 hours. The reaction mixture was cooled and decomposed by the addition of water and the precipitate filtered. The precipitate was washed with tetrahydrofuran and the combined filtrate and washings evaporated to a solid. The solid was dissolved in water and ammonium chloride added. The precipitated oil was extracted with dichloromethane, dried over anhydrous magnesium sulphate and evaporated to leave a solid which was recrystallised from acetonitrile to give 0.91 g of the title compound, m.p. 127.5°-133° C., identical with material prepared by an alternative route described in U.K. Pat. No. 1,285,025.

1. temperatureheated
2. temperatureunder reflux for 5 hours
3. temperatureThe reaction mixture was cooled
4. filtrationthe precipitate filtered
5. washThe precipitate was washed with tetrahydrofuran
6. customthe combined filtrate and washings evaporated to a solid
7. dissolutionThe solid was dissolved in water
8. additionammonium chloride added
9. extractionThe precipitated oil was extracted with dichloromethane
10. dry with materialdried over anhydrous magnesium sulphate
11. customevaporated
12. customto leave a solid which
13. customwas recrystallised from acetonitrile