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1H-1,2,4-Triazole → HCID 14403430、化合物

HRID 1650733
ノート
印刷プレビュー

反応式

HRID 1650733 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]=[CH:10][C:11]1([C:14]2([S:17][CH2:18][CH2:19][CH3:20])[CH2:16][CH2:15]2)[CH2:13][O:12]1.[NH:21]1[CH:25]=[N:24][CH:23]=[N:22]1.CC(C)([O-])C.[K+]>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1/[CH:9]=[CH:10]/[C:11]([C:14]1([S:17][CH2:18][CH2:19][CH3:20])[CH2:16][CH2:15]1)([OH:12])[CH2:13][N:21]1[CH:25]=[N:24][CH:23]=[N:22]1
参加物反応条件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 23665647Potassium tert-butoxideHCID 540874812-(2,4-Dichlorophenylethenyl)-2-(1-propylmercaptocyclopropyl) oxirane

生成物 1

HCID 14403430HCID 14403430、化合物収率 26%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
80 °C

実験手順

A solution of 38.2 g (0.12 mol) of 2-(2,4-dichlorophenylethenyl)-2-(1-propylmercaptocyclopropyl) oxirane in 30 ml of dimethylformamide is added dropwise under a nitrogen atmosphere and with stirring at 80° C. to a mixture of 24 g (0.35 mol) of 1,2,4-triazole, 2.7 g (0.02 mol) of potassium tert.-butoxide and 50 ml of dimethylformamide. The mixture is stirred at 80° C. for 6 hours, then the solvent is removed under reduced pressure, and the residue is taken up in ethyl acetate/toluene, washed with water, dried over sodium sulphate and concentrated under reduced pressure. The residue which remains is chromatographed on silica gel using chloroform as the eluant. In this manner, 12.1 g (26% of theory) of trans-4-(2,4-dichlorophenyl)-2-(1-propylmercaptocyclopropyl)1-(1,2,4-triazol-1-yl)-but-3-en-2-ol are obtained in the form of an oily product.

後処理

  1. customthe solvent is removed under reduced pressure
  2. washwashed with water
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue which remains is chromatographed on silica gel

出典と根拠

ORDレコード
ord-ba115882bbec43588ffe3edd859fcbaa
出典データセット
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04925865

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート