HCID 2799775、化合物 → Imidazo[1,5-a]pyridine-3-acetonitrile
反応式
[C:1]([CH2:3][C:4]([NH:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=1)=O)#[N:2]>P(Cl)(Cl)(Cl)=O>[C:1]([CH2:3][C:4]1[N:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]2=[CH:7][N:6]=1)#[N:2]参加物
3
実験手順
Heat under reflux for 0.5 hours a mixture of 9 gm (0.06 mol) 2-cyano-N-(2-pyridylmethyl)acetamide and 100 ml phosphorous oxychloride. Cool the reaction mixture to room temperature and remove the phosphorus oxychloride under reduced pressure. Partition the residue between chloroform and a solution of sodium bicarbonate. Separate the chloroform layer and dry over anhydrous potassium carbonate. Filter and remove the chloroform under reduced pressure. Chromatograph the resulting residue on silica gel using ethyl acetate-chloroform to give the desired product, 3-cyanomethyl imidazo[1,5-a]pyridine, as determined by IR, NMR and elemental analysis, m.p. 64°-66°.
後処理
- temperatureHeat
- temperatureunder reflux for 0.5 hours
- customremove the phosphorus oxychloride under reduced pressure
- customPartition the residue between chloroform
- customSeparate the chloroform layer
- dry with materialdry over anhydrous potassium carbonate
- filtrationFilter
- customremove the chloroform under reduced pressure
出典と根拠
- ORDレコード
- ord-416af44747254a58ba5d0a71748e93d0
- 出典データセット
- uspto-grants-1982_11
- 特許番号
- US04361567
反応ノート
読み込み中…