2-Bromoethanol → 2-(4-Bromo-2-(trifluoromethyl)phenoxy)-ethanol

HRID 2079533노트

반응식

HRID 2079533 반응식
Br[CH2:2][CH2:3][OH:4].[Br:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([C:13]([F:16])([F:15])[F:14])[CH:7]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C.C(OCC)(=O)C>[Br:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:2][CH2:3][OH:4])=[C:8]([C:13]([F:14])([F:15])[F:16])[CH:7]=1

참가 물질

6

반응물 3

HCID 108982-Bromoethanol2회HCID 11430Potassium CarbonateHCID 142784o-Cresol, 4-bromo-alpha,alpha,alpha-trifluoro-

생성물 1

HCID 576575832-(4-Bromo-2-(trifluoromethyl)phenoxy)-ethanol

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

2-Bromoethanol (23.3 g) was added to a mixture of 4-bromo-2-(trifluoromethyl)-phenol (30 g) and potassium carbonate (34.4 g) in acetonitrile (200 ml). The above mixture was refluxed for 8 hours then another portion of 2-bromoethanol (8 g) was added and the reflux continued for another 6 hours. After diluting with ethyl acetate (500 ml), the mixture was washed with water (300 ml) then 0.1 M sodium hydroxide (200 ml). Organic layer was dried over magnesium sulphate, solvent removed under reduced pressure, the residue was taken into heptane by heat, 2-(4-bromo-2-(trifluoromethyl)-phenoxy)-ethanol crystalised and collected by filtration (17 g).

후처리

  1. temperatureThe above mixture was refluxed for 8 hours
  2. washthe mixture was washed with water (300 ml)
  3. dry with materialOrganic layer was dried over magnesium sulphate, solvent
  4. customremoved under reduced pressure
  5. temperatureby heat
  6. custom2-(4-bromo-2-(trifluoromethyl)-phenoxy)-ethanol crystalised
  7. filtrationcollected by filtration (17 g)

출처 및 근거

ORD 기록
ord-75c1a8ec3ef34072aefb62563ffc1e9e
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932251B2

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