Potassium Carbonate → 3-(2-Chloro-4-trifluoromethoxyphenoxy)propanol

HRID 229350노트

반응식

HRID 229350 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]([F:12])([F:11])[F:10])[CH:5]=[CH:4][C:3]=1[OH:13].Br[CH2:15][CH2:16][CH2:17][OH:18].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]([F:11])([F:12])[F:10])[CH:5]=[CH:4][C:3]=1[O:13][CH2:15][CH2:16][CH2:17][OH:18]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 123083-Bromo-1-propanolHCID 130447832-Chloro-4-(trifluoromethoxy)phenol

생성물 1

HCID 685273763-(2-Chloro-4-trifluoromethoxyphenoxy)propanol수율 96%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 2-chloro-4-trifluoromethoxyphenol (16.4 g, 0.077 mole) in 100 mL of acetonitrile was added 3-bromopropanol (12.87 g, 0.092 mole) and potassium carbonate (21.33 g, 0.154 mole). The resulted solution was refluxed at 75° C.-80° C. overnight. The solvent was then evaporated. The residue was dissolved in 100 mL of ethyl acetate and washed with 100 mL of H2O. The organic layer was separated, dried over MgSO4, filtered and the organic solvent was evaporated to yield 20 g of the product.

후처리

  1. temperatureThe resulted solution was refluxed at 75° C.-80° C. overnight
  2. customThe solvent was then evaporated
  3. dissolutionThe residue was dissolved in 100 mL of ethyl acetate
  4. washwashed with 100 mL of H2O
  5. customThe organic layer was separated
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customthe organic solvent was evaporated

출처 및 근거

ORD 기록
ord-e272d54994bb40d983421826a14aa4f3
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563792B2

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