1,8-Diazabicyclo(5.4.0)undec-7-ene → 1-Methoxy-4-(pentafluoro-lambda~6~-sulfanyl)benzene

HRID 2080937

반응식

HRID 2080937 반응식
[F:1][S:2]([F:13])([F:12])([F:11])([F:10])[C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[CH2:14]1CCN2C(=NCCC2)CC1>C(=O)(OC)OC.CC(=O)OCC>[CH3:14][O:9][C:6]1[CH:7]=[CH:8][C:3]([S:2]([F:10])([F:11])([F:12])([F:13])[F:1])=[CH:4][CH:5]=1

참가 물질

5

반응물 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 27792034-Hydroxyphenylsulfur pentafluoride

생성물 1

HCID 596421411-Methoxy-4-(pentafluoro-lambda~6~-sulfanyl)benzene수율 41.4%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 12021Dimethyl Carbonate용매

실험 절차

5.00 g of 4-pentafluorosulfanylphenol were dissolved in 50.00 g of dimethyl carbonate and 3.46 g of DBU were added. The mixture was boiled under reflux for 10 hours, then allowed to cool and diluted with 200 ml of EA. Subsequently, the mixture was washed twice with 100 ml each time of a 5% aqueous HCl solution, then with 100 ml of a 5% aqueous NaOH solution. Drying was effected over MgSO4 and the solvent was removed under reduced pressure. Chromatography on silica gel using 1:1 DIP/HEP afforded 2.2 g of a colorless oil.

후처리

  1. temperatureunder reflux for 10 hours
  2. temperatureto cool
  3. washSubsequently, the mixture was washed twice with 100 ml each time of a 5% aqueous HCl solution
  4. customDrying
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-ef5689f16adc46ed85f114b2649afa4f
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932416B2

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