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Water → 1-Acetoxy-1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-ethane

HRID 1702765
ノート
印刷プレビュー

反応式

HRID 1702765 の反応式
[C:1]([O-:4])(=[O:3])[CH3:2].[Na+].[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[CH:14](O)[CH2:15][N:16]1[CH:20]=[N:19][CH:18]=[N:17]1.O>C(OC(=O)C)(=O)C>[C:1]([O:4][CH:14]([C:8]1[CH:9]=[CH:10][C:11]([Cl:13])=[CH:12][C:7]=1[Cl:6])[CH2:15][N:16]1[CH:20]=[N:19][CH:18]=[N:17]1)(=[O:3])[CH3:2]
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 962WaterHCID 517045Sodium AcetateHCID 66285758905-18-3

生成物 1

HCID 205251601-Acetoxy-1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-ethane収率 43%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

A pinch of sodium acetate was added to 25.8 g (0.1 mol) of 1-(2,4-dichlorophenyl)-1-hydroxy-2-(1,2,4-triazol-1-yl)-ethane in 100 ml of acetic anhydride and the mixture was then kept for 10 hours at a temperature of 100° C. Thereafter the solution was cooled and stirred into 1,000 ml of water. A smeary, crystalline mass precipitated, which was taken up in chloroform. The chloroform solution was washed with sodium bicarbonate and water, dried over sodium sulphate and concentrated by distilling off the solvent in vacuo. The residue crystallized on adding petroleum ether. 13 g (43% of theory) of 1-acetoxy-1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-ethane of melting point 92°-96° C. were obtained.

後処理

  1. temperatureThereafter the solution was cooled
  2. customA smeary, crystalline mass precipitated
  3. washThe chloroform solution was washed with sodium bicarbonate and water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated
  6. distillationby distilling off the solvent in vacuo
  7. customThe residue crystallized
  8. additionon adding petroleum ether

出典と根拠

ORDレコード
ord-66cab67954b64cff9c26dd71340fa034
出典データセット
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04349556

反応ノート

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