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Ammonium Chloride → HCID 117759923、化合物

HRID 1049553
ノート
印刷プレビュー

反応式

HRID 1049553 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 2724141Tetrabutylammonium FluorideHCID 131736026HCID 131736026、化合物

生成物 1

HCID 117759923HCID 117759923、化合物収率 89.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-f9df91f0fb404e34b2d8ab2e64870382
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09382188B2

反応ノート

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