反応 #2222836
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07964625B2
反応条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 100 mmol 2-fluoroaniline and 50 mmol diethyl malonate were put together and stirred overnight at 170° C. The formed ethanol was distilled off directly (100 mmol≡6.6 mL) on a stream of nitrogen. N1,N3-di(2-fluoro-phenyl)-malonamide was formed as one solid block. The reaction was cooled and EtOAc was added. The product had to be crushed with a mortar, because it resembled very hard brick. The crushed material was stirred in EtOAc and filtered. EtOAc added was added twice and the mixture was stirred and filtered each time. 9.9 g N1,N3-di(2-fluoro-phenyl)-malonamide was obtained (yield 68.2%, purity 99.3%) The formed ethanol was distilled off directly (100 mmol≡6.6 mL) on a stream of nitrogen
ソース ID: ord-a3ac3fdfcef742979ab7488da0fb4d6d