反应详情

In a Parr bottle were combined 5% Pd/C (10 g of 50% water-wet) and 60 g of 8-fluoro-5- (p-fluorophenyl)-2-carbobenzoxy-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]-indole (60 g, 0.143 mole) in 400 ml ethyl acetate and 100 ml methanol and the mixture hydrogenated at 44-80 psig for 4 hours. Catalyst was recovered by filtration and the filtrate evaporated to solids in vacuo. The residue taken into CH2Cl2, carbon treated, dried (Na2SO4) and CH2Cl2 displaced with hexane by distillation to a final pot temperature of 70° C. The white, crystalline product was recovered by filtration, 35.6 g, m.p. 126°-129° C.

1. filtrationCatalyst was recovered by filtration
2. customthe filtrate evaporated to solids in vacuo
3. additiontreated
4. dry with materialdried (Na2SO4) and CH2Cl2
5. distillationdisplaced with hexane by distillation to a final pot temperature of 70° C
6. filtrationThe white, crystalline product was recovered by filtration, 35.6 g, m.p. 126°-129° C.