2-bromoethanamine;hydrochloride

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

実験手順: A solution of 5.0 g (0.015 mol) of 5-amino-N,N-diethyl-2H[1]benzothiopyrano[4,3,2-cd]indazole-2-ethanamine and 9.2 g (0.045 mol) of 2-bromoethylamine, hydrochloride in 50 ml of EtOH was heated under reflux for four days and allowed to cool to room temperature. The solid was collected and recrystallized from MeOH to give 2.6 g of product, mp 263° C. dec. under reflux for four days The solid was collected recrystallized from MeOH

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

実験手順: To a solution of 2-bromoethylamine hydrochloride (25 g: a product of Tokyo Kasei Kogyo Co., Ltd.) and triethylamine (34 ml) in methylene chloride (450 ml), benzyloxycarbonyl chloride (19 ml) was added dropwise over a period of 20 minutes and the mixture was agitated at room temeprature for 19 hours. The resulting reaction mixture was washed with water, with saturated aqueous sodium bicarbonate solution and with saturated aqueous sodium chloride succeedingly, whereupon the separated organic layer was dried and, then, removed off the solvent by distilling it of under reduced pressure. The residue was cooled with ice and the crystals were collected by filtration and washed with hexane, whereby the above-identified compound was obtained (29.4 g). The resulting reaction mixture was washed with water, with saturated aqueous sodium bicarbonate solution and with saturated aqueous sodium chloride succeedingly whereupon the separated organic layer was dried removed off the solvent by distilling it of under reduced pressure The residue was cooled with ice the crystals were collected by filtration washed with hexane, whereby the above-identified compound was obtained (29.4 g)

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

実験手順: To 30 ml of ethanol, 1.2 g of 4-mercaptophenol, 2.1 g of 2-bromoethylamine hydrochloride and 1.4 g of potassium carbonate were added, followed by stirring for 3 hours at room temperature. Water was added, and the resulting mixture was extracted with ethyl ether. The extract was dried over MgSO4 and the ethyl ether was distilled off under reduced pressure, whereby 1.7 g of the compound (7) were obtained (yield: stoichiometric). the resulting mixture was extracted with ethyl ether The extract was dried over MgSO4 the ethyl ether was distilled off under reduced pressure

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

実験手順: A solution of 5.0 g (0.015 mol) of 5-amino-N,N-diethyl-2H[1]benzothiopyrano[4,3,2-cd]indazole-2-ethanamine and 9.2 g (0.045 mol) of 2-bromoethylamine, hydrochloride in 50 ml of EtOH was heated under reflux for four days and allowed to cool to room temperature. The solid was collected and recrystallized from MeOH to give 2.6 g of product, mp 263° C. dec. under reflux for four days The solid was collected recrystallized from MeOH

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

実験手順: A solution of 5.0 g (0.015 mol) of 5-amino-N,N-diethyl-2H[1]benzothiopyrano[4,3,2-cd]indazole-2-ethanamine and 9.2 g (0.045 mol) of 2-bromoethylamine, hydrochloride in 50 ml of EtOH was heated under reflux for four days and allowed to cool to room temperature. The solid was collected and recrystallized from MeOH to give 2.6 g of product, mp 263° C. dec. under reflux for four days The solid was collected recrystallized from MeOH

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

実験手順: To a solution of 2-bromoethylamine hydrochloride (25 g: a product of Tokyo Kasei Kogyo Co., Ltd.) and triethylamine (34 ml) in methylene chloride (450 ml), benzyloxycarbonyl chloride (19 ml) was added dropwise over a period of 20 minutes and the mixture was agitated at room temeprature for 19 hours. The resulting reaction mixture was washed with water, with saturated aqueous sodium bicarbonate solution and with saturated aqueous sodium chloride succeedingly, whereupon the separated organic layer was dried and, then, removed off the solvent by distilling it of under reduced pressure. The residue was cooled with ice and the crystals were collected by filtration and washed with hexane, whereby the above-identified compound was obtained (29.4 g). The resulting reaction mixture was washed with water, with saturated aqueous sodium bicarbonate solution and with saturated aqueous sodium chloride succeedingly whereupon the separated organic layer was dried removed off the solvent by distilling it of under reduced pressure The residue was cooled with ice the crystals were collected by filtration washed with hexane, whereby the above-identified compound was obtained (29.4 g)

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

実験手順: To 30 ml of ethanol, 1.2 g of 4-mercaptophenol, 2.1 g of 2-bromoethylamine hydrochloride and 1.4 g of potassium carbonate were added, followed by stirring for 3 hours at room temperature. Water was added, and the resulting mixture was extracted with ethyl ether. The extract was dried over MgSO4 and the ethyl ether was distilled off under reduced pressure, whereby 1.7 g of the compound (7) were obtained (yield: stoichiometric). the resulting mixture was extracted with ethyl ether The extract was dried over MgSO4 the ethyl ether was distilled off under reduced pressure

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

実験手順: A solution of 5.0 g (0.015 mol) of 5-amino-N,N-diethyl-2H[1]benzothiopyrano[4,3,2-cd]indazole-2-ethanamine and 9.2 g (0.045 mol) of 2-bromoethylamine, hydrochloride in 50 ml of EtOH was heated under reflux for four days and allowed to cool to room temperature. The solid was collected and recrystallized from MeOH to give 2.6 g of product, mp 263° C. dec. under reflux for four days The solid was collected recrystallized from MeOH