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1H-1,2,4-Triazole → Benzyl 4-(1,2,4-triazol-1-yl)butyrate

HRID 962778
ノート
印刷プレビュー

反応式

HRID 962778 の反応式
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:13][CH2:14][CH2:15][C:16]([O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17]>C(#N)C>[N:1]1([CH2:13][CH2:14][CH2:15][C:16]([O:18][CH2:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)=[O:17])[CH:5]=[N:4][CH:3]=[N:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 3832489Benzyl 4-bromobutanoate

生成物 1

HCID 10490579Benzyl 4-(1,2,4-triazol-1-yl)butyrate収率 81.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4.7 g of 1,2,4-triazole and 9.5 g of potassium carbonate were added to a solution of 15 g of benzyl 4-bromobutyrate in 150 ml of acetonitrile. The mixture was refluxed by heating, for 1 hour. The reaction mixture was concentrated under reduced pressure. To the residue was added 30 ml of methylene chloride. The insolubles were collected by filtration and washed. The filtrate and the washings were combined and purified by silica gel column chromatography (eluant: methylene chloride/methanol=50/1) to obtain 11.6 g of benzyl 4-(1,2,4-triazol-1-yl)butyrate as a colorless oily substance.

後処理

  1. temperatureThe mixture was refluxed
  2. temperatureby heating, for 1 hour
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionTo the residue was added 30 ml of methylene chloride
  5. filtrationThe insolubles were collected by filtration
  6. washwashed
  7. custompurified by silica gel column chromatography (eluant: methylene chloride/methanol=50/1)

出典と根拠

ORDレコード
ord-b33dd683fa5741a99375809a84768d1b
出典データセット
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05760058

反応ノート

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