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2,6-Lutidine → HCID 131736006、化合物

HRID 1049450
ノート
印刷プレビュー

反応式

HRID 1049450 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[C:11]([OH:17])=[CH:12][C:13]([OH:16])=[CH:14][CH:15]=1.FC(F)(F)S(O[Si:24]([CH:31]([CH3:33])[CH3:32])([CH:28]([CH3:30])[CH3:29])[CH:25]([CH3:27])[CH3:26])(=O)=O.CC1C=CC=C(C)N=1.[Cl-].[NH4+]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[C:11]([OH:17])=[CH:12][C:13]([O:16][Si:24]([CH:31]([CH3:33])[CH3:32])([CH:28]([CH3:30])[CH3:29])[CH:25]([CH3:27])[CH3:26])=[CH:14][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 79372,6-LutidineHCID 25517Ammonium ChlorideHCID 2724529Triisopropylsilyl trifluoromethanesulfonateHCID 117759897HCID 117759897、化合物

生成物 1

HCID 131736006HCID 131736006、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Under a nitrogen atmosphere, to a solution of 2′-fluoro-5′-methoxybiphenyl-2,4-diol (10.6 g) in toluene (80 mL) were added triisopropylsilyl trifluoromethanesulfonate (18 mL) and 2,6-dimethylpyridine (8.0 mL) at −15° C., and the mixture was stirred for 3 hr. To the reaction mixture was added 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 (10.5 g) as a pale-yellow 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-43234d701220409692c47b789fb2b3c9
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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