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Water → HCID 117759962, 화합물

HRID 1049554
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HRID 1049554 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 117759923HCID 117759923, 화합물HCID 117760149HCID 117760149, 화합물

생성물 1

HCID 117759962HCID 117759962, 화합물수율 82.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

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-d1339c9f7bcd470d83aa760e2a6eddb8
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382188B2

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