5-Benzyl-10-oxo-10,11-dihydro-5H-dibenz[b,f]azepine

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 149.7 g (0.5 mole) of 5-benzyl-5,11-dihydro-10H-dibenz[b,f]azepin-10-one (vide British Pat. No. 961 444),27 ml of hydrogen fluoride, 125 g of sulphur tetrafluoride and 400 ml of methylene chloride is heated in a steel autocalve for 16 hours to 70° C. After the mixture has cooled, the bulk of the liquid constituents are filtered off with suction. Then water and aqueous ammonia solution are added until the pH of the aqueous phase is 9-10. The organic phase is separated, washed three times with water, diluted with 200 ml of benzene and concentrated in a rotary evaporator. The black residue is dissolved in methylene chloride and the solution is filtered through 700 g of silica gel (particle size 0.063-0.2 mm) with methylene chloride as eluant. The filtrate is concentrated, the residue dissolved in 1.5 liters of benzene and stirred for 30 minutes with 500 g of magnesium silicate gel. The mixture is filtered and 500 g of magnesium silicate gel are again added to the filtrate. After repeated filtration, the solution is concentrated in vacuo and the black residue is chromatographed over 800 g of silica gel (particle size 0.063-0.2 mm) with hexane/benzene (2:1) as eluant. The homogeneous fractions are combined and concentrated to yield the 5-benzyl-10-fluoro-5H-dibenz[b,f]azepine as a light yellow oil. After the mixture has cooled the bulk of the liquid constituents are filtered off with suction Then water and aqueous ammonia solution are added until the pH of the aqueous phase The organic phase is separated washed three times with water diluted with 200 ml of benzene concentrated in a rotary evaporator The black residue is dissolved in methylene chloride the solution is filtered through 700 g of silica gel (particle size 0.063-0.2 mm) with methylene chloride as eluant The filtrate is concentrated the residue dissolved in 1.5 liters of benzene The mixture is filtered 500 g of magnesium silicate gel are again added to the filtrate filtration the solution is concentrated in vacuo the black residue is chromatographed over 800 g of silica gel (particle size 0.063-0.2 mm) with hexane/benzene (2:1) as eluant concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 149.7 g (0.5 mole) of 5-benzyl-5,11-dihydro-10H-dibenz[b,f]azepin-10-one (vide British Pat. No. 961 444),27 ml of hydrogen fluoride, 125 g of sulphur tetrafluoride and 400 ml of methylene chloride is heated in a steel autocalve for 16 hours to 70° C. After the mixture has cooled, the bulk of the liquid constituents are filtered off with suction. Then water and aqueous ammonia solution are added until the pH of the aqueous phase is 9-10. The organic phase is separated, washed three times with water, diluted with 200 ml of benzene and concentrated in a rotary evaporator. The black residue is dissolved in methylene chloride and the solution is filtered through 700 g of silica gel (particle size 0.063-0.2 mm) with methylene chloride as eluant. The filtrate is concentrated, the residue dissolved in 1.5 liters of benzene and stirred for 30 minutes with 500 g of magnesium silicate gel. The mixture is filtered and 500 g of magnesium silicate gel are again added to the filtrate. After repeated filtration, the solution is concentrated in vacuo and the black residue is chromatographed over 800 g of silica gel (particle size 0.063-0.2 mm) with hexane/benzene (2:1) as eluant. The homogeneous fractions are combined and concentrated to yield the 5-benzyl-10-fluoro-5H-dibenz[b,f]azepine as a light yellow oil. After the mixture has cooled the bulk of the liquid constituents are filtered off with suction Then water and aqueous ammonia solution are added until the pH of the aqueous phase The organic phase is separated washed three times with water diluted with 200 ml of benzene concentrated in a rotary evaporator The black residue is dissolved in methylene chloride the solution is filtered through 700 g of silica gel (particle size 0.063-0.2 mm) with methylene chloride as eluant The filtrate is concentrated the residue dissolved in 1.5 liters of benzene The mixture is filtered 500 g of magnesium silicate gel are again added to the filtrate filtration the solution is concentrated in vacuo the black residue is chromatographed over 800 g of silica gel (particle size 0.063-0.2 mm) with hexane/benzene (2:1) as eluant concentrated