17-chloro-4-methyl-13-oxa-4-azatetracyclo[12.4.0.02,6.07,12]octadeca-1(14),2(6),7,9,11,15,17-heptaen-3-one

反応条件: temp:98.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Anhydrous aluminium chloride (5 g) was added to a reaction mixture containing 3-(5-chloro-2-phenoxyphenyl)-1-methylpyrrolidine-2,4-dione (1 g) in monochlorobenzene (1 mL) at ambient temperature. The reaction mixture was stirred at about 98° C. for about 1 hour, then cooled to ambient temperature. A mixture of water and concentrated hydrochloric acid (50 mL:5 mL) was added slowly. The contents were stirred for about 30 minutes. Hexane (50 mL) was added. The contents were stirred for about 1 hour, filtered, washed with hexane (15 mL) and dried in air at about 30° C. for about 15 hours to obtain 11-chloro-2-methyl-2,3-dihydro-1H-dibenzo [2,3:6,7] oxepino [4,5-c]pyrrol-1-one. cooled to ambient temperature was added slowly The contents were stirred for about 30 minutes The contents were stirred for about 1 hour filtered washed with hexane (15 mL) dried in air at about 30° C. for about 15 hours

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

実験手順: Anhydrous aluminium chloride (5 g) was added to a reaction mixture containing 3-(5-chloro-2-phenoxyphenyl)-1-methylpyrrolidine-2,4-dione (1 g) in 1,2-dichlorobenzene (5 mL) at ambient temperature. The reaction mixture was stirred at about 85° C. for about 2 hours and 30 minutes, then cooled to ambient temperature. A mixture of water and concentrated hydrochloric acid (50 mL:5 mL) was added dropwise. The contents were stirred for about 30 minutes. Hexane (10 mL) was added. The contents were stirred for about 15 minutes, filtered, washed with hexane (10 mL) and dried in air at about 30° C. for about 15 hours followed by further drying at about 50° C. under reduced pressure to obtain 11-chloro-2-methyl-2,3-dihydro-1H-dibenzo [2,3:6,7]oxepino[4,5-c]pyrrol-1-one. cooled to ambient temperature was added dropwise The contents were stirred for about 30 minutes The contents were stirred for about 15 minutes filtered washed with hexane (10 mL) dried in air at about 30° C. for about 15 hours by further drying at about 50° C. under reduced pressure

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

実験手順: Anhydrous aluminium bromide (2.5 g) was added to a reaction mixture containing 3-(5-chloro-2-phenoxyphenyl)-1-methylpyrrolidine-2,4-dione (1 g) in 1,2-dichlorobenzene (4 mL) at ambient temperature. The reaction mixture was stirred at about 85° C. for about 9 hours, then cooled to ambient temperature. A mixture of water and concentrated hydrochloric acid (50 mL:5 mL) was added slowly. The contents were stirred for about 30 minutes. Hexane (10 mL) was added. The contents were stirred for about 1 hour, filtered, washed with hexane (10 mL) and dried in air at about 30° C. for about 15 hours to obtain 11-chloro-2-methyl-2,3-dihydro-1H-dibenzo [2,3:6,7]oxepino[4,5-c]pyrrol-1-one. cooled to ambient temperature was added slowly The contents were stirred for about 30 minutes The contents were stirred for about 1 hour filtered washed with hexane (10 mL) dried in air at about 30° C. for about 15 hours

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

実験手順: Anhydrous aluminium bromide (2.5 g) was added to a reaction mixture containing 3-(5-chloro-2-phenoxyphenyl)-1-methylpyrrolidine-2,4-dione (1 g) in 1,2-dichlorobenzene (4 mL) at ambient temperature. The reaction mixture was stirred at about 85° C. for about 9 hours, then cooled to ambient temperature. A mixture of water and concentrated hydrochloric acid (50 mL:5 mL) was added slowly. The contents were stirred for about 30 minutes. Hexane (10 mL) was added. The contents were stirred for about 1 hour, filtered, washed with hexane (10 mL) and dried in air at about 30° C. for about 15 hours to obtain 11-chloro-2-methyl-2,3-dihydro-1H-dibenzo [2,3:6,7]oxepino[4,5-c]pyrrol-1-one. cooled to ambient temperature was added slowly The contents were stirred for about 30 minutes The contents were stirred for about 1 hour filtered washed with hexane (10 mL) dried in air at about 30° C. for about 15 hours

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

実験手順: Anhydrous aluminium bromide (2.5 g) was added to a reaction mixture containing 3-(5-chloro-2-phenoxyphenyl)-1-methylpyrrolidine-2,4-dione (1 g) in 1,2-dichlorobenzene (4 mL) at ambient temperature. The reaction mixture was stirred at about 85° C. for about 9 hours, then cooled to ambient temperature. A mixture of water and concentrated hydrochloric acid (50 mL:5 mL) was added slowly. The contents were stirred for about 30 minutes. Hexane (10 mL) was added. The contents were stirred for about 1 hour, filtered, washed with hexane (10 mL) and dried in air at about 30° C. for about 15 hours to obtain 11-chloro-2-methyl-2,3-dihydro-1H-dibenzo [2,3:6,7]oxepino[4,5-c]pyrrol-1-one. cooled to ambient temperature was added slowly The contents were stirred for about 30 minutes The contents were stirred for about 1 hour filtered washed with hexane (10 mL) dried in air at about 30° C. for about 15 hours