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Hydrochloric Acid → HCID 178509695、化合物

HRID 431998
ノート
印刷プレビュー

反応式

HRID 431998 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[CH:11][N:12](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:13]=2)[CH:6]=[CH:7][CH:8]=1)#[N:2].Cl>O1CCCC1>[C:1]([C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[CH:11][NH:12][CH:13]=2)[CH:6]=[CH:7][CH:8]=1)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 219426904-(3-cyanophenyl)-1-trityl-1H-imidazole

生成物 1

HCID 178509695HCID 178509695、化合物収率 72%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 4-(3-cyanophenyl)-1-trityl-1H-imidazole (0.07 g, 0.17 mmol) in tetrahydrofuran (1.36 mL) was treated with 2N hydrochloric acid (0.68 mL) and the resulting mixture was heated at reflux for 45 minutes. After cooling the reaction mixture was concentrated in vacuo and the residue dissolved in dichloromethane (20 mL). The organic phase was successively washed with 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL). The organic solution was dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. Silica gel chromatography of the residues using 3% methanol in dichloromethane afforded 0.02 g (72%) of 4-(3-cyanophenyl)imidazole as a white solid.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 45 minutes
  3. temperatureAfter cooling the reaction mixture
  4. concentrationwas concentrated in vacuo
  5. dissolutionthe residue dissolved in dichloromethane (20 mL)
  6. washThe organic phase was successively washed with 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL)
  7. dry with materialThe organic solution was dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-5bf36b5f3bef435fa49030720762c082
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06660753B2

反応ノート

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