Phosphorus oxychloride → 4-(Imidazo[1,5-a]pyridin-5-yl)benzonitrile

HRID 568527ノート

反応式

HRID 568527 の反応式
C([NH:5][C:6]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[N:19]3[CH:20]=[N:21][CH:22]=[C:18]3[CH:17]=[CH:16][CH:15]=2)=[CH:10][CH:9]=1)=O)(C)(C)C.P(Cl)(Cl)(Cl)=O>C1(C)C=CC=CC=1>[C:6]([C:8]1[CH:9]=[CH:10][C:11]([C:14]2[N:19]3[CH:20]=[N:21][CH:22]=[C:18]3[CH:17]=[CH:16][CH:15]=2)=[CH:12][CH:13]=1)#[N:5]

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 136882255-(p-Tert-butylaminocarbonylphenyl)imidazo[1,5-a]pyridine

生成物 1

HCID 136882234-(Imidazo[1,5-a]pyridin-5-yl)benzonitrile

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 0.1 g of 5-(p-tert-butylaminocarbonylphenyl)imidazo[1,5-a]pyridine in 3 ml of toluene is treated with 40 μl of phosphorus oxychloride at 90° for 5 h. The solvent is evaporated and the residue is redissolved in 30 ml of chloroform at 0°. An ice-cold ammonium hydroxide solution is added and the organic phase is separated, dried over sodium sulfate and evaporated. The residue is chromatographed on silica with ethyl acetate to yield the title compound, m.p. 117°-118°.

後処理

  1. customThe solvent is evaporated
  2. dissolutionthe residue is redissolved in 30 ml of chloroform at 0°
  3. additionAn ice-cold ammonium hydroxide solution is added
  4. customthe organic phase is separated
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue is chromatographed on silica with ethyl acetate

出典と根拠

ORDレコード
ord-b45c7ce9d2b5413f9c61bc132cf03377
出典データセット
uspto-grants-1988_03
特許番号
US04728645

反応ノート

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