Water → 2-methoxy-3,5-dimethylbenzaldehyde

HRID 1067405ノート

反応式

HRID 1067405 の反応式
C[O:2][C:3]1[CH:8]=[CH:7][C:6]([CH3:9])=[CH:5][C:4]=1[CH3:10].[CH3:11][O:12][CH:13](Cl)Cl.O>C(Cl)Cl.[Ti](Cl)(Cl)(Cl)Cl>[CH3:11][O:12][C:13]1[C:4]([CH3:10])=[CH:5][C:6]([CH3:9])=[CH:7][C:8]=1[CH:3]=[O:2]

参加物

6

反応物 3

HCID 962WaterHCID 21004Methane, dichloromethoxy-HCID 812212,4-Dimethylanisole

生成物 1

HCID 47704302-methoxy-3,5-dimethylbenzaldehyde収率 98%

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-methoxy-2,4-dimethylbenzene (8.00 g, 58.7 mmol) and 1,1-dichloromethyl methyl ether (7.40 g, 64.7 mmol) in methylene chloride (30 mL) was added titanium tetrachloride (20.0 g, 105 mmol) at 0° C. and the mixture was stirred at that temperature for 20 minutes. This reaction mixture was poured into iced water and the organic layer was taken, washed with saturated aqueous sodium hydrogen carbonate solution, dried over MgSO4, and filtered. The filtrate was concentrated under reduced pressure to provide 9.40 g of the title compound. Yield 98%. Oil.

後処理

  1. washwashed with saturated aqueous sodium hydrogen carbonate solution
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-3c050f13aeb741f3b98f7fd9f083b323
出典データセット
uspto-grants-2001_06
特許番号
US06248766B1

反応ノート

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