반응 #84387

ord-6d14eed077b7449f9c742e1b9f77be85

시약

없음

용매

반응 조건

온도
55°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to rt
  2. 2
    여과filtered
  3. 3
    농축the filtrate was concentrated in vacuo
  4. 4
    기타The 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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09434695B2uspto-grants-2016_09