反应详情

Add a 1M benzene solution of sodium bis(2-methoxyethoxy)aluminum hydroxide (Red-Al®)(5.3 ml.) dropwise with stirring at room temperature to a solution of dl-6-(dimethylaminoacetyl)-5,6,7,12-tetrahydro-5,12-methanodibenz[c,f]azocine (2.8 g. of the free base) in benzene (27 ml.) over 0.5 hours. Reflux for 2 hours, cool, stir at room temperature then quench by careful addition of saturated aqueous ammonium chloride solution (1.85 ml.) dropwise with stirring. Filter and evaporate the filtrate in vacuo. Dissolve the residue in methylene chloride, wash with water, brine then dry and evaporate the solvent in vacuo to obtain 2.79 g. of the free base of the title product as a viscous oil. Treat the free base with two equivalents of fumaric acid in acetone to obtain the title product as the difumarate salt, m.p. 169°-171.5° C.

1. temperatureReflux for 2 hours
2. temperaturecool
3. customthen quench by careful addition of saturated aqueous ammonium chloride solution (1.85 ml.) dropwise
4. stirringwith stirring
5. filtrationFilter
6. customevaporate the filtrate in vacuo
7. dissolutionDissolve the residue in methylene chloride
8. washwash with water, brine
9. customthen dry
10. customevaporate the solvent in vacuo
11. customto obtain 2.79 g