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Water → 5-Bromo-2-methoxy-3-(trifluoromethyl)benzaldehyde

HRID 385013
ノート
印刷プレビュー

反応式

HRID 385013 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:11]([F:14])([F:13])[F:12])[C:5]([OH:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].[C:15](=O)([O-])[O-].[K+].[K+].COS(=O)(=O)OC.O>CN(C)C=O>[Br:1][C:2]1[CH:3]=[C:4]([C:11]([F:12])([F:13])[F:14])[C:5]([O:10][CH3:15])=[C:6]([CH:9]=1)[CH:7]=[O:8]
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 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 27792785-Bromo-2-hydroxy-3-(trifluoromethyl)benzaldehyde

生成物 1

HCID 840703065-Bromo-2-methoxy-3-(trifluoromethyl)benzaldehyde収率 98.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

5-bromo-2-hydroxy-3-trifluoromethylbenzaldehyde (63.98 g) was dissolved in N,N-dimethylformamide (130 mL), and potassium carbonate (65.79 g) and dimethylsulfuric acid (31.6 mL) were added to the solution under water cooling, and then the mixture was stirred at room temperature for 3 hours. Water was added to the reaction solution, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (66.19 g) as a brown crystal.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with 1N hydrochloric acid and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-d155db9a08a245189aab07163777c986
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367843B2

反応ノート

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