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

HRID 385013
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HRID 385013 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 27792785-Bromo-2-hydroxy-3-(trifluoromethyl)benzaldehyde

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d155db9a08a245189aab07163777c986
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367843B2

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