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

Imidazole → [3-(1H-Imidazol-1-yl)phenyl](2,4,6-trimethylphenyl)methanone

HRID 1380300
ノート
印刷プレビュー

反応式

HRID 1380300 の反応式
[H-].[Na+].[NH:3]1[CH:7]=[CH:6][N:5]=[CH:4]1.F[C:9]1[CH:10]=[C:11]([CH:23]=[CH:24][CH:25]=1)[C:12]([C:14]1[C:19]([CH3:20])=[CH:18][C:17]([CH3:21])=[CH:16][C:15]=1[CH3:22])=[O:13]>CN(C)P(=O)(N(C)C)N(C)C>[N:3]1([C:9]2[CH:10]=[C:11]([CH:23]=[CH:24][CH:25]=2)[C:12]([C:14]2[C:15]([CH3:22])=[CH:16][C:17]([CH3:21])=[CH:18][C:19]=2[CH3:20])=[O:13])[CH:7]=[CH:6][N:5]=[CH:4]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 795ImidazoleHCID 24758Sodium hydrideHCID 13457470HCID 13457470、化合物

生成物 1

HCID 13247704[3-(1H-Imidazol-1-yl)phenyl](2,4,6-trimethylphenyl)methanone収率 80.4%

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

反応条件

温度
40 °C

実験手順

To a suspension of 2.9 g of sodium hydride (60% dispersion in mineral oil) in 50 ml of hexamethylphosphoric triamide is added 5.3 g of imidazole over a 30 minute period under heating at 40° C. After the addition is complete, the mixture is stirred at room temperature for an hour. To the reaction mixture is added 16.6 g of 3-fluoro-2',4',6'-trimethylbenzophenone and the mixture is stirred at 70° C. for 24 hours. The reaction solution is poured into ice-cold water and extracted with ethyl acetate. The ethyl acetate layer is washed with water, dried and concentrated. The residue is recrystallized from a mixture of toluene and isopropyl ether to give 16 g of 3-(1-imidazolyl)-2',4',6'-trimethylbenzophenone as white crystals, melting at 134°-136° C.

後処理

  1. additionAfter the addition
  2. stirringthe mixture is stirred at 70° C. for 24 hours
  3. additionThe reaction solution is poured into ice-cold water
  4. extractionextracted with ethyl acetate
  5. washThe ethyl acetate layer is washed with water
  6. customdried
  7. concentrationconcentrated
  8. customThe residue is recrystallized from a mixture of toluene and isopropyl ether

出典と根拠

ORDレコード
ord-f4bf90626fa74498b55225cb5a9c8dc3
出典データセット
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04581369

反応ノート

読み込み中…

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