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Ammonium Chloride → HCID 117759923, 화합물

HRID 1049553
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HRID 1049553 반응식
[C:1]([O:5][C:6]1[CH:11]=[C:10]([O:12][Si](C(C)C)(C(C)C)C(C)C)[CH:9]=[CH:8][C:7]=1[C:23]1[CH:28]=[C:27]([O:29][CH3:30])[CH:26]=[CH:25][C:24]=1[F:31])([CH3:4])([CH3:3])[CH3:2].[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[Cl-].[NH4+]>C1COCC1>[C:1]([O:5][C:6]1[CH:11]=[C:10]([OH:12])[CH:9]=[CH:8][C:7]=1[C:23]1[CH:28]=[C:27]([O:29][CH3:30])[CH:26]=[CH:25][C:24]=1[F:31])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 2724141Tetrabutylammonium FluorideHCID 131736026HCID 131736026, 화합물

생성물 1

HCID 117759923HCID 117759923, 화합물수율 89.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Under a nitrogen atmosphere, to a solution of ((2-(tert-butoxy)-2′-fluoro-5′-methoxy-[1,1′-biphenyl]-4-yl)oxy)triisopropylsilane (96.2 mg) in THF (1.44 mL) was added a 1 M solution (431 μL) of tetrabutylammonium fluoride in THF at room temperature, and the mixture was stirred for 1 hr. The reaction mixture was poured into saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (56.1 mg) as a colorless oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-f9df91f0fb404e34b2d8ab2e64870382
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382188B2

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