Phosphorus sulfide (P2S5) → Benzenecarbothioamide, 4-(diethylamino)-
反応式
[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]参加物
4
反応条件
- 温度
- 55 °C
実験手順
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%).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-6d14eed077b7449f9c742e1b9f77be85
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434695B2
反応ノート
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