反应 #1822057
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05185337
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To 7 g of (+)-8,9-difluoro-2-(S)-methyl-6-oxo-1,2-dihydro-6H-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid obtained in Example 5 were added 21 g of aminopyrrolidine dihydrochloride, 40 ml of 1,8-diazabicyclo[5,4,0]-7-undecene (DBU) and 70 ml of hexamethylphosphoric triamide, and allowed to react in an oil bath at 120°-130° C. for 2 hours. The solvent was evaporated off under reduced pressure, and the residue was dissolved in 100 ml of 2% aqueous hydrochloric acid. Insoluble matters were filtered off, the filtrate was concentrated, and the residue was recrystallized from ethanol-water to obtain (+)-8-fluoro-2-methyl-9-(3-amino-1-pyrrolidyl)-6-oxo-1,2-dihydro-6H-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid hydrochloride. to react in an oil bath at 120°-130° C. for 2 hours The solvent was evaporated off under reduced pressure the residue was dissolved in 100 ml of 2% aqueous hydrochloric acid Insoluble matters were filtered off the filtrate was concentrated the residue was recrystallized from ethanol-water
来源 ID: ord-1933d3e55a42466b8b4629691ebb9dff