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

Sodium hydride → 1-(1H-1,2,4-triazol-1-yl)-2-(4-chlorophenoxymethyl)-3,3-dimethylbutene

HRID 615067
ノート
印刷プレビュー

反応式

HRID 615067 の反応式
[H-].[Na+].[N:3]1([CH2:8]P(=O)(OCC)OCC)[CH:7]=[N:6][CH:5]=[N:4]1.[CH3:17][C:18]([CH3:31])([C:20](=O)[CH2:21][O:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=1)[CH3:19].C1OCCOCCOCCOCCOC1>C(COC)OC>[N:3]1([CH:8]=[C:20]([CH2:21][O:22][C:23]2[CH:24]=[CH:25][C:26]([Cl:29])=[CH:27][CH:28]=2)[C:18]([CH3:31])([CH3:17])[CH3:19])[CH:7]=[N:6][CH:5]=[N:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 24758Sodium hydrideHCID 3633615-Crown-5HCID 905182-Butanone, 1-(4-chlorophenoxy)-3,3-dimethyl-HCID 15145771Diethyl [(1H-1,2,4-triazol-1-yl)methyl]phosphonate

生成物 1

HCID 543931591-(1H-1,2,4-triazol-1-yl)-2-(4-chlorophenoxymethyl)-3,3-dimethylbutene

試薬・触媒・溶媒 1

HCID 8071
1,2-Dimethoxyethane
溶媒
2 回

実験手順

15 g of sodium hydride in the form of a 55% dispersion in oil are added under nitrogen to 150 ml of 1,2-dimethoxyethane. Then a solution of 69 g (0.315 mole) of diethyl (1H-1,2,4-triazol-1-yl)methylphosphonate, 68 g (0.3 mole) of 2,2-dimethyl-4-(4-chlorophenoxy)butan-3-one and a trace of 15-crown-5 in 500 ml of dimethoxyethane are added dropwise. The reaction mixture is stirred for about 10 hours and, after the dropwise addition of ice/water, extracted with methylene chloride. The combined extracts are washed with water, dried over sodium sulfate, filtered and concentrated. The oily residue is purified by column chromatography over silica gel with a 4:2:2:2 mixture of toluene/cyclohexane/diethyl ether/dichloromethane as eluant, affording the product in the form of a yellow oil.

後処理

  1. extractionextracted with methylene chloride
  2. washThe combined extracts are washed with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe oily residue is purified by column chromatography over silica gel with a 4:2:2:2 mixture of toluene/cyclohexane/diethyl ether/dichloromethane as eluant
  7. customaffording the product in the form of a yellow oil

出典と根拠

ORDレコード
ord-3ca6835f18eb423db1c78c83a7b9bce0
出典データセット
uspto-grants-1985_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04497647

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