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4-Chloro-6,7-dimethoxyquinoline → HCID 22132715、化合物

HRID 1857124
ノート
印刷プレビュー

反応式

HRID 1857124 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[CH:4][CH:3]=1.[CH:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18][C:17]=1[C:26]([C:28]1[CH:33]=[CH:32][C:31]([OH:34])=[CH:30][CH:29]=1)=[O:27]>>[CH3:13][O:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][C:8]=1[O:14][CH3:15])[N:5]=[CH:4][CH:3]=[C:2]2[O:34][C:31]1[CH:32]=[CH:33][C:28]([C:26]([C:17]2[CH:18]=[CH:19][C:20]3[C:25](=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH:16]=2)=[O:27])=[CH:29][CH:30]=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

3

反応物 2

HCID 4596104-Chloro-6,7-dimethoxyquinolineHCID 15640646HCID 15640646、化合物

生成物 1

HCID 22132715HCID 22132715、化合物収率 23%

反応条件

温度
180 °C

実験手順

4-Chloro-6,7-dimethoxyquinoline (112 mg) and 4-hydroxyphenyl 2-naphthyl ketone (124 mg) obtained in Example 36 were mixed and stirred at 180° C. for 30 minutes. The reaction mixture was partitioned between saturated aqueous sodium hydrogen carbonate and chloroform, and then the chloroform layer was dried with anhydrous magnesium sulfate. After removing the solvent by reduced-pressure distillation, a portion (50 mg) of the resulting residue (227 mg) was purified by thin layer chromatography on silica gel eluting with chloroform/ethyl acetate (5/1) to obtain 11 mg of the title compound (yield: 23%).

後処理

  1. customThe reaction mixture was partitioned between saturated aqueous sodium hydrogen carbonate and chloroform
  2. dry with materialthe chloroform layer was dried with anhydrous magnesium sulfate
  3. customAfter removing the solvent
  4. distillationby reduced-pressure distillation
  5. customa portion (50 mg) of the resulting residue (227 mg) was purified by thin layer chromatography on silica gel eluting with chloroform/ethyl acetate (5/1)

出典と根拠

ORDレコード
ord-11442cdf0a4e4bae8d3eeab06a566ca6
出典データセット
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06143764

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