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Water → HCID 117759962、化合物

HRID 1049554
ノート
印刷プレビュー

反応式

HRID 1049554 の反応式
[C:1]([O:5][C:6]1[CH:11]=[C:10]([OH:12])[CH:9]=[CH:8][C:7]=1[C:13]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][C:14]=1[F:21])([CH3:4])([CH3:3])[CH3:2].Br[CH2:23][C:24]1[CH:25]=[C:26]([CH:30]([CH:37]2[CH2:39][CH2:38]2)[CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:27]=[CH:28][CH:29]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[C:1]([O:5][C:6]1[CH:11]=[C:10]([O:12][CH2:23][C:24]2[CH:25]=[C:26]([CH:30]([CH:37]3[CH2:38][CH2:39]3)[CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:27]=[CH:28][CH:29]=2)[CH:9]=[CH:8][C:7]=1[C:13]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][C:14]=1[F:21])([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

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 117759923HCID 117759923、化合物HCID 117760149HCID 117760149、化合物

生成物 1

HCID 117759962HCID 117759962、化合物収率 82.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Under a nitrogen atmosphere, to a solution of 2-(tert-butoxy)-2′-fluoro-5′-methoxy-[1,1′-biphenyl]-4-ol (96.1 mg) in DMF (3.31 mL) were added ethyl 3-(3-(bromomethyl)phenyl)-3-cyclopropylpropanoate (124 mg) and potassium carbonate (91 mg) at room temperature, and the mixture was stirred for 3 hr. The reaction mixture was poured into water, 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 (142 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-d1339c9f7bcd470d83aa760e2a6eddb8
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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