Phosphorus sulfide (P2S5) → Benzenecarbothioamide, 4-(diethylamino)-
반응식
[CH2:1]([N:3]([CH2:13][CH3:14])[C:4]1[CH:12]=[CH:11][C:7]([C:8]([NH2:10])=O)=[CH:6][CH:5]=1)[CH3:2].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:16]>C1COCC1>[CH2:1]([N:3]([CH2:13][CH3:14])[C:4]1[CH:12]=[CH:11][C:7]([C:8](=[S:16])[NH2:10])=[CH:6][CH:5]=1)[CH3:2]참가 물질
4
반응 조건
- 온도
- 55 °C
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%).
후처리
- temperaturecooled to rt
- filtrationfiltered
- concentrationthe filtrate was concentrated in vacuo
- customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:1)
출처 및 근거
- ORD 기록
- ord-6d14eed077b7449f9c742e1b9f77be85
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09434695B2
반응 노트
불러오는 중…