Ammonia → 1-Phenylisoquinoline-5-acetonitrile

HRID 1156906ノート

反応式

HRID 1156906 の反応式
[Na].N.[C:3]1([C:9]2[C:18]3[C:13](=[C:14](Cl)[CH:15]=[CH:16][CH:17]=3)[CH:12]=[CH:11][N:10]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:20](#[N:22])[CH3:21]>[Fe](Cl)(Cl)Cl>[C:3]1([C:9]2[C:18]3[CH:17]=[CH:16][CH:15]=[C:14]([CH2:21][C:20]#[N:22])[C:13]=3[CH:12]=[CH:11][N:10]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 222Ammonia2 回HCID 6342AcetonitrileHCID 5360545SodiumHCID 128518471-Phenyl-5-chloroisoquinoline

生成物 1

HCID 205339011-Phenylisoquinoline-5-acetonitrile

試薬・触媒・溶媒 1

HCID 24380Iron chloride (FeCl3)触媒

実験手順

Metallic sodium (1.15 g) was added to 100 ml of liquid ammonia, and 1.3 g of acetonitrile and 2.39 g of 1-phenyl-5-chloroisoquinoline were added to the solution. A small amount of iron trichloride was added, and the reaction was performed for 5 hours. After the reaction, ammonia was distilled off, and ice water was carefully added to the residue. The resulting oily product was extracted with ether, and dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was chromatographed to afford 1-phenylisoquinoline-5-acetonitrile as an oil.

後処理

  1. additionwere added to the solution
  2. distillationwas distilled off
  3. additionice water was carefully added to the residue
  4. extractionThe resulting oily product was extracted with ether
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off
  7. customthe residue was chromatographed

出典と根拠

ORDレコード
ord-b1ecab48abdb44b48aa9f4814e16224f
出典データセット
uspto-grants-1982_06
特許番号
US04337256

反応ノート

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