HCID 2799775、化合物 → Imidazo[1,5-a]pyridine-3-acetonitrile

HRID 2199048ノート

反応式

HRID 2199048 の反応式
[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

  1. temperatureHeat
  2. temperatureunder reflux for 0.5 hours
  3. customremove the phosphorus oxychloride under reduced pressure
  4. customPartition the residue between chloroform
  5. customSeparate the chloroform layer
  6. dry with materialdry over anhydrous potassium carbonate
  7. filtrationFilter
  8. 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

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