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Water → alpha-Methoxy-beta-[4-(4-trifluoromethylphenoxy)phenoxy]propane

HRID 224219
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HRID 224219 반응식
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:20]=[CH:19][C:6]([O:7][C:8]2[CH:18]=[CH:17][C:11]([O:12][CH:13]([CH3:16])[CH2:14][OH:15])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.[Na].[CH3:24]I.O>O1CCOCC1>[CH3:24][O:15][CH2:14][CH:13]([O:12][C:11]1[CH:17]=[CH:18][C:8]([O:7][C:6]2[CH:19]=[CH:20][C:3]([C:2]([F:21])([F:22])[F:1])=[CH:4][CH:5]=2)=[CH:9][CH:10]=1)[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 5360545SodiumHCID 128048852-{4-[4-(Trifluoromethyl)phenoxy]phenoxy}propan-1-ol

생성물 1

HCID 23332249alpha-Methoxy-beta-[4-(4-trifluoromethylphenoxy)phenoxy]propane수율 67%

시약·촉매·용매 1

HCID 312751,4-Dioxane
용매

실험 절차

6 g of β-[4-(4-trifluoromethylphenoxy)phenoxy]propanol was dissolved in 30 ml of dioxane and 0.46 g of sodium was added to the solution. The mixture was then heated for 3 hours while refluxing. 3.1 g of methyl iodide was added thereto and the resulting mixture was heated for 6 hours while refluxing. The reaction mixture was then poured into an appropriate amount of water and extracted with diethyl ether. The extract was washed with water and dried over anhydrous sodium sulfate. The ether was removed by distillation and the residue was distilled under reduced pressure to obtain 4.2 g of the desired product having a boiling point of 160° to 165° C./2 mmHg.

후처리

  1. temperatureThe mixture was then heated for 3 hours
  2. temperaturewhile refluxing
  3. temperaturethe resulting mixture was heated for 6 hours
  4. temperaturewhile refluxing
  5. extractionextracted with diethyl ether
  6. washThe extract was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe ether was removed by distillation
  9. distillationthe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-061c08d0d11e49a8b07107610448537e
출처 데이터셋
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04231787

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