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Water → (4-Methoxyphenyl)(2-methyl-3-nitrophenyl)methanone

HRID 1090069
ノート
印刷プレビュー

反応式

HRID 1090069 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[CH3:5][C:6]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=[CH:11][C:7]=1[C:8](Cl)=[O:9].[C:18]1([O:24][CH3:25])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O>C(Cl)Cl>[CH3:25][O:24][C:18]1[CH:23]=[CH:22][C:21]([C:8]([C:7]2[C:6]([CH3:5])=[C:14]([N+:15]([O-:17])=[O:16])[CH:13]=[CH:12][CH:11]=2)=[O:9])=[CH:20][CH:19]=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 962WaterHCID 7519AnisoleHCID 6451240Aluminum(III) ChlorideHCID 121948722-Methyl-3-nitrobenzoyl chloride

生成物 1

HCID 14535915(4-Methoxyphenyl)(2-methyl-3-nitrophenyl)methanone収率 68.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒
2 回

実験手順

To a suspension of 95.6 g (0.716 mole) of aluminum chloride in 500 ml of methylene dichloride was added, rapidly and with stirring, a solution of 110.1 g (0.551 mole) of 2-methyl-3-nitrobenzoyl chloride in 400 ml of methylene dichloride. The mixture was then transferred to an addition funnel, added with stirring to a solution of 59.8 g (0.551 mole) of anisole over a thirty minute period, and the reaction mixture then heated under reflux for two hours. The mixture was decomposed by the careful addition, with stirring, of 1 liter of water and then filtered. The organic layer was separated from the aqueous layer, dried and taken to dryness, and the residue recrystallized from ethyl acetate to give 102.9 g of 3-(4-methoxybenzoyl)-2-methylnitrobenzene, m.p. 110°-113° C.

後処理

  1. additionwas added
  2. customThe mixture was then transferred to an addition funnel
  3. additionadded
  4. temperaturethe reaction mixture then heated
  5. temperatureunder reflux for two hours
  6. additionThe mixture was decomposed by the careful addition
  7. filtrationfiltered
  8. customThe organic layer was separated from the aqueous layer
  9. customdried
  10. customthe residue recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-65c07704b08641b2a1cb3a0862da7961
出典データセット
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05081122

反応ノート

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