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1,2-Dimethoxyethane → HCID 15947801、化合物

HRID 1673019
ノート
印刷プレビュー

反応式

HRID 1673019 の反応式
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]([C:19]2[C:24]([Cl:25])=[CH:23][CH:22]=[CH:21][C:20]=2[Cl:26])[N:9]([C:11]2[CH:16]=[CH:15][C:14](Br)=[CH:13][C:12]=2[Cl:18])[CH:10]=1)=[O:5])[CH3:2].[CH3:27][S:28]([C:31]1[CH:32]=[C:33](B(O)O)[CH:34]=[CH:35][CH:36]=1)(=[O:30])=[O:29].C([O-])([O-])=O.[K+].[K+].COCCOC>CCOC(C)=O.O>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]([C:19]2[C:24]([Cl:25])=[CH:23][CH:22]=[CH:21][C:20]=2[Cl:26])[N:9]([C:11]2[CH:16]=[CH:15][C:14]([C:35]3[CH:34]=[CH:33][CH:32]=[C:31]([S:28]([CH3:27])(=[O:30])=[O:29])[CH:36]=3)=[CH:13][C:12]=2[Cl:18])[CH:10]=1)=[O:5])[CH3:2]
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

7

反応物 4

HCID 80711,2-DimethoxyethaneHCID 11430Potassium CarbonateHCID 27735423-(Methylsulfonyl)phenylboronic acidHCID 592404041-(4-Bromo-2-chloro-phenyl)-2-(2,6-dichloro-phenyl)-1H-imidazole-4-carboxylic acid ethyl ester

生成物 1

HCID 15947801HCID 15947801、化合物収率 79%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

To a 2 L round bottom flask attached with condenser column and magnetic stir bar was added 1-(4-Bromo-2-chloro-phenyl)-2-(2,6-dichloro-phenyl)-1H-imidazole-4-carboxylic acid ethyl ester (21.1 g, 44.5 mmol), 3-methylsulfonylphenyl boronic acid (9.78 g, 48.9 mmol), PdCl2dppf (1.09 g, 3 mol %), K2CO3 (18.9 g, 137 mmol), 1,2-dimethoxyethane (250 mL) and H2O (50 mL). The reaction solution was allowed to stir at 80° C. for 2.5 hrs. The reaction solution was diluted with EtOAc (150 mL) and filtered through a Celite padded Buchner funnel to remove spent Pd. The filtrate was transferred to a separatory funnel and washed with aq NH4Cl (300 mL) and aq NaCl (200 mL). The organic phase was dried over Na2SO4, filtered, concentrated on the rotavapor and chromatographed through a 300 g SiO2 column using a mobile phase gradient of 3% EtOAc to 100% EtOAc to afford 19.3 g (79% yield) of the title compound. MS (ESI) 549.3, 551.3, 553.3 [M+H]+.

後処理

  1. customTo a 2 L round bottom flask attached with condenser
  2. filtrationfiltered through a Celite
  3. customto remove
  4. customThe filtrate was transferred to a separatory funnel
  5. washwashed with aq NH4Cl (300 mL) and aq NaCl (200 mL)
  6. dry with materialThe organic phase was dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated on the rotavapor
  9. customchromatographed through a 300 g SiO2 column

出典と根拠

ORDレコード
ord-6a5cb4977c2b4ed09537eab6db91c0b3
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07998995B2

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