반응 #84387
ord-6d14eed077b7449f9c742e1b9f77be85
용매
반응 조건
온도
55°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도cooled to rt
- 2여과filtered
- 3농축the filtrate was concentrated in vacuo
- 4기타The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:1)
실험 절차
To a solution of 4-(diethylamino)benzamide (5.66 g, 29.43 mmol) in THF (80 mL) was added P2S5 (9.81 g, 44.14 mmol) at 50° C. over a period of 1 h. The mixture was heated at 55° C. for 8 h, then cooled to rt, filtered and the filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:1) to give the title compound as a yellow solid (1.23 g, 20%).