ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1H-1,2,4-Triazole → 4-(2,4-Dichlorophenyl)-3,3-dimethyl-2-(1,2,4-triazol-1-ylmethyl)-1-(1,2,4-triazol-1-yl)-2-butanol

HRID 1608245
ノート
印刷プレビュー

反応式

HRID 1608245 の反応式
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.[Na].[Cl:7][C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[CH2:15][C:16]([C:19]1([CH2:22][N:23]2[CH:27]=[N:26][CH:25]=[N:24]2)[CH2:21][O:20]1)([CH3:18])[CH3:17]>C(O)CC>[Cl:7][C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[CH2:15][C:16]([CH3:18])([CH3:17])[C:19]([CH2:22][N:23]1[CH:27]=[N:26][CH:25]=[N:24]1)([OH:20])[CH2:21][N:1]1[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 5360545SodiumHCID 133403832-(2,4-Dichlorophenyl-tert.-butyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane

生成物 1

HCID 133403844-(2,4-Dichlorophenyl)-3,3-dimethyl-2-(1,2,4-triazol-1-ylmethyl)-1-(1,2,4-triazol-1-yl)-2-butanol収率 18.8%

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒2 回

実験手順

3.7 g (52.6 mmol) of 1,2,4-triazole are added to a solution of 0.11 g (47 mmol) of sodium in 30 ml of n-propanol at room temperature, while stirring. The mixture is heated to the reflux temperature and a solution of 15.4 g (47 mmol) of 2-(2,4-dichlorophenyl-tert.-butyl)-2-(1,2,4-triazol-1-yl-methyl)-oxirane in 20 ml of n-propanol is added. The reaction mixture is heated under reflux for 15 hours and then cooled and poured onto water. It is extracted with methylene chloride and the organic phase is dried over sodium sulphate and concentrated. The residue is purified by column chromatography (silica gel; ethyl acetate:cyclohexane=3:1). 3.5 g (18.8% of theory) of 4-(2,4-dichlorophenyl)-3,3-dimethyl-2-(1,2,4-triazol-1-yl-methyl)-1-(1,2,4-triazol-1-yl)-2-butanol of melting point 126° C. are obtained.

後処理

  1. temperatureThe mixture is heated to the reflux temperature
  2. temperatureThe reaction mixture is heated
  3. temperatureunder reflux for 15 hours
  4. temperaturecooled
  5. additionpoured onto water
  6. extractionIt is extracted with methylene chloride
  7. dry with materialthe organic phase is dried over sodium sulphate
  8. concentrationconcentrated
  9. customThe residue is purified by column chromatography (silica gel; ethyl acetate:cyclohexane=3:1)

出典と根拠

ORDレコード
ord-efceda746449462e967eaf047fa8f7b1
出典データセット
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04870092

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート