4,5-DIHYDRO-1H-BENZO[E][1,4]DIAZEPIN-2(3H)-ONE

反应条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The mixture of 2,4-dichloro-6-methyl-quinoline (422 mg, 2 mmol), 1,3,4,5-tetrahydro-2H-1,4-benzodiazepin-2-one (298 mg, 2 mmol) and n-butyl alcohol (15 mL) was heated with stirring in a 20 mL microwave process vial for 3 hours at 160° C. under microwave irradiation. After cooling, the solvent was removed in vacuo and the residue was purified by column chromatography on silica gel (methanol/dichloromethane, 1:20) to give the product. MS obsd. (ESI+) [(M+H)+] 338. was heated After cooling the solvent was removed in vacuo the residue was purified by column chromatography on silica gel (methanol/dichloromethane, 1:20) to give the product

反应条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The mixture of 2,4-dichloro-6-methyl-quinoline (422 mg, 2 mmol), 1,3,4,5-tetrahydro-2H-1,4-benzodiazepin-2-one (298 mg, 2 mmol) and n-butyl alcohol (15 mL) was heated with stirring in a 20 mL microwave process vial for 3 hours at 160° C. under microwave irradiation. After cooling, the solvent was removed in vacuo and the residue was purified by column chromatography on silica gel (methanol/dichloromethane, 1:20) to give the product. MS obsd. (ESI+) [(M+H)+] 338. was heated After cooling the solvent was removed in vacuo the residue was purified by column chromatography on silica gel (methanol/dichloromethane, 1:20) to give the product

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

实验步骤: To a solution of 2-oxo-1,2,3,5-tetrahydro-benzo[e][1,4]diazepine-4-carboxylic acid tert-butyl ester (300 mg, 1.14 mmol) in dry DCM (10 mL) was added trifluoroacetic acid (3.42 mL, 3 mL/mmol. The reaction mixture was stirred at r.t. for 2 h. After completion of the reaction as confirmed by TLC, excess of trifluoroacetic acid and DCM were removed under vacuo to afford trifluoroacetic acid salt of 1,3,4,5-tetrahydro-benzo[e][1,4]diazepin-2-one (295 mg, 93%) as a gummy solid. The crude compound was used as such without further purification for the next step. After completion of the reaction were removed under vacuo

反应条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The mixture of 2,4-dichloro-6-methyl-quinoline (422 mg, 2 mmol), 1,3,4,5-tetrahydro-2H-1,4-benzodiazepin-2-one (298 mg, 2 mmol) and n-butyl alcohol (15 mL) was heated with stirring in a 20 mL microwave process vial for 3 hours at 160° C. under microwave irradiation. After cooling, the solvent was removed in vacuo and the residue was purified by column chromatography on silica gel (methanol/dichloromethane, 1:20) to give the product. MS obsd. (ESI+) [(M+H)+] 338. was heated After cooling the solvent was removed in vacuo the residue was purified by column chromatography on silica gel (methanol/dichloromethane, 1:20) to give the product