Chloroform → HCID 90405189、化合物
反応式
[CH3:1][O:2][C:3]1[C:11]([CH3:12])=[CH:10][CH:9]=[C:8]2[C:4]=1[CH:5]=[C:6]([C:13]([NH2:15])=O)[NH:7]2.P(Cl)(Cl)(Cl)=O.C(Cl)(Cl)Cl>O>[CH3:1][O:2][C:3]1[C:11]([CH3:12])=[CH:10][CH:9]=[C:8]2[C:4]=1[CH:5]=[C:6]([C:13]#[N:15])[NH:7]2参加物
5
実験手順
A mixture of 79 mg of 4-methoxy-5-methyl-1H-indole-2-carboxamide (0.39 mmol), 0.19 mL of phosphorus oxychloride (2 mmol) and 1.5 mL of chloroform was refluxed for 2 hs. Then cooled solution was poured into 10 mL of water and stirred for 1 hr. After separation the organic layer was dried over sodium sulfate and concentrated. The residue was purified on silica gel column using hexane-ethyl acetate 5:1 to afford 51 mg of 4-methoxy-5-methyl-1H-indole-2-carbonitrile.
後処理
- temperaturewas refluxed for 2 hs
- customAfter separation the organic layer
- dry with materialwas dried over sodium sulfate
- concentrationconcentrated
- customThe residue was purified on silica gel column
出典と根拠
- ORDレコード
- ord-737521f778834f9fa40a31bbfdfb8b35
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09216993B2
反応ノート
読み込み中…