Dimethyl Sulfate → 3-Bromo-4,5-dimethoxybenzaldehyde

HRID 488830

反応式

HRID 488830 の反応式
[Br:1][C:2]1[C:3]([OH:12])=[C:4]([O:10][CH3:11])[CH:5]=[C:6]([CH:9]=1)[CH:7]=[O:8].[C:13](=O)([O-])[O-].[K+].[K+].COS(OC)(=O)=O>CC(C)=O.C(OCC)(=O)C>[Br:1][C:2]1[CH:9]=[C:6]([CH:5]=[C:4]([O:10][CH3:11])[C:3]=1[O:12][CH3:13])[CH:7]=[O:8]

参加物

6

反応物 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 180995-Bromovanillin

生成物 1

HCID 813793-Bromo-4,5-dimethoxybenzaldehyde収率 89%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 5-bromovanillin (2.00 g, 8.65 mmol) in acetone (50 mL) was added potassium carbonate (1.4 g, 10.38 mmol) and dimethylsulfate (1 mL, 10.38 mmol). The solution was stirred at room temperature for 16 hours. The reaction mixture was diluted with ethyl acetate and the organic layer was washed successively with water and brine, dried over anhydrous magnesium sulfate, filtered and evaporated to afford 1.88 g of 3-bromo-4,5-dimethoxybenzaldehyde (89%).

後処理

  1. washthe organic layer was washed successively with water and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-c76798833fc6472b8a037b56a9eede7b
出典データセット
uspto-grants-2005_12
特許番号
US06974826B2

関連ノート

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