1,5-dihydro-3-benzazepine-2,4-dione

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Here, 1,3,4,5-tetrahydro-2H-3-benzazepin-2,4-dione (3.5 g, 0.020 mol) is suspended in dimethylformamide (30 ml) and potassium tert. butoxide (2.5 g) is added with stirring. After 10 minutes the resulting solution is added dropwise, while cooling with ice, to 1-bromo-3-chloro-propane (3.5 ml) in dimethylformamide (20 ml). After one hour it is poured onto ice water. After a short time the greasy precipitate crystallizes. The precipitate is suction filtered, dissolved in acetone, reprecipitated with water, suction filtered and dried. After 10 minutes the resulting solution is added dropwise After one hour it is poured onto ice water After a short time the greasy precipitate crystallizes filtered dissolved in acetone reprecipitated with water, suction filtered dried

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A quantity of 3.5 gm (0.020 mol) of 1,3,4,5-tetrahydro-2H-3-benzazepin-2,4-dione is suspended in 30 ml of dimethylformamide and mixed with 2.5 gm of potassium tert.butoxide with stirring. After ten minutes, the solution obtained is added dropwise to 3.5 ml of 1-bromo-3-chloropropane in 20 ml of dimethylformamide while being cooled with ice. After one hour the mixture is poured onto ice water. A short time later the greasy precipitate crystallizes. The precipitate is subjected to suction filtration, dissolved in acetone, precipitated again with water, suction filtered, and dried. After ten minutes the solution obtained while being cooled with ice After one hour the mixture is poured onto ice water A short time later the greasy precipitate crystallizes The precipitate is subjected to suction filtration dissolved in acetone precipitated again with water, suction filtered dried

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of 1,5-dihydro-benzo[d]azepine-2,4-dione (9.3 g) in toluene (250 ml) borane-methylsulfide complex (20 ml) was added dropwise under nitrogen atmosphere, then the mixture was heated at reflux for 4 h. MeOH (20 ml) was added dropwise and the mixture refluxed for additional 1 h, then cooled to room temperature. A 10% solution of anidrous HCl in ethyl ether (50 ml) was added and the solid precipitate was filtered off, washed with ethyl ether and desiccated under reduced pressure to afford the title compound as a white solid (7.6 g, 78% yield). was added dropwise under nitrogen atmosphere the mixture was heated at reflux for 4 h the mixture refluxed for additional 1 h the solid precipitate was filtered off washed with ethyl ether

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Bromo-1H-benzo[d]azepin-2-ylamine hydrobromide (41.2 g) was dissolved in 600 ml of H2O that was previously heated to 85° C. Sodium acetate trihydrate (18.5 g) was added portion wise and the solution was heated to 90° C. for 3 h. Cooling to room temperature caused the precipitation of a white solid that was filtered-off, washed with water and desiccated under reduced pressure to afford the title compound (20.4 g, 90% yield). the solution was heated to 90° C. for 3 h Cooling to room temperature the precipitation of a white solid washed with water

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Here, 1,3,4,5-tetrahydro-2H-3-benzazepin-2,4-dione (3.5 g, 0.020 mol) is suspended in dimethylformamide (30 ml) and potassium tert. butoxide (2.5 g) is added with stirring. After 10 minutes the resulting solution is added dropwise, while cooling with ice, to 1-bromo-3-chloro-propane (3.5 ml) in dimethylformamide (20 ml). After one hour it is poured onto ice water. After a short time the greasy precipitate crystallizes. The precipitate is suction filtered, dissolved in acetone, reprecipitated with water, suction filtered and dried. After 10 minutes the resulting solution is added dropwise After one hour it is poured onto ice water After a short time the greasy precipitate crystallizes filtered dissolved in acetone reprecipitated with water, suction filtered dried