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Anisole → 3,4-Dichloro-4'-methoxybenzophenone

HRID 1857191
ノート
印刷プレビュー

反応式

HRID 1857191 の反応式
[C:1]1([O:7][CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:9][C:10]1[CH:11]=[C:12]([CH:16]=[CH:17][C:18]=1[Cl:19])[C:13](Cl)=[O:14].FC(F)(F)S([O-])(=O)=O.[Yb+3].FC(F)(F)S([O-])(=O)=O.FC(F)(F)S([O-])(=O)=O>[N+](C)([O-])=O>[CH3:8][O:7][C:1]1[CH:6]=[CH:5][C:4]([C:13]([C:12]2[CH:16]=[CH:17][C:18]([Cl:19])=[C:10]([Cl:9])[CH:11]=2)=[O:14])=[CH:3][CH:2]=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 7519AnisoleHCID 76403Benzoyl chloride, 3,4-dichloro-HCID 2733225Ytterbium triflate

生成物 1

HCID 27581233,4-Dichloro-4'-methoxybenzophenone収率 10%

試薬・触媒・溶媒 1

HCID 6375Nitromethane溶媒

反応条件

温度
60 °C

実験手順

To commercially available nitromethane (10 ml) were added commercially available anisole (1.081 g), commercially available 3,4-dichlorobenzoyl chloride (2.095 g) and commercially available ytterbium(III) trifluoromethanesulfonate (620 mg), and the admixture was stirred at 60° C. for 8 hours. The reaction mixture was partitioned between water and chloroform, and the chloroform layer was then dried with anhydrous magnesium sulfate. After removing the solvent by reduced-pressure distillation, the resulting residue was purified by column chromatography on silica gel eluting with hexane/ethyl acetate to obtain 270 mg of the title compound (yield: 10%).

後処理

  1. customThe reaction mixture was partitioned between water and chloroform
  2. dry with materialthe chloroform layer was then dried with anhydrous magnesium sulfate
  3. customAfter removing the solvent
  4. distillationby reduced-pressure distillation
  5. customthe resulting residue was purified by column chromatography on silica gel eluting with hexane/ethyl acetate

出典と根拠

ORDレコード
ord-873b20d8028e43e3be8e2dcc019cc66d
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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