Dichloromethane → 3-Phenylpropanethioamide
反応式
[C:1]1([CH2:7][CH2:8][C:9]([NH2:11])=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:21])=CC=1.CCCCCC.C(Cl)Cl>C1(C)C=CC=CC=1.C(O)(=O)C>[C:1]1([CH2:7][CH2:8][C:9]([NH2:11])=[S:21])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1参加物
7
実験手順
To a solution of 3-phenylpropionamide (1.653 g, 6.827 mmol) in toluene (20 mL) was added Lawesson's reagent (0.716 g, 1.77 mmol). The reaction was refluxed overnight, cooled to room temperature and concentrated yielding an orange oil. Flash chromatography of this oil (1:1 hexane:methylene chloride with 1% acetic acid) yielded 3-phenylthiopropionamide (0.070 g) as a white solid: mp 82°-83° C.; 1HNMR (DMSO d6) 300 mHz 9.35 (br s, 1 H), 9.15 (br s, 1 H), 7.34-7.10 (m, 2 H), 2.95 (t, J=8.48 Hz, 2 H), 2.72 (t, J=8.48 Hz, 2 H).
後処理
- temperatureThe reaction was refluxed overnight
- concentrationconcentrated
- customyielding an orange oil
出典と根拠
- ORDレコード
- ord-7dec5218e5674c959072d8306e0cf727
- 出典データセット
- uspto-grants-1997_09
- 特許番号
- US05668161
反応ノート
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