Potassium Carbonate → HCID 21911050, 화합물

HRID 1245434

반응식

HRID 1245434 반응식
F[C:2]1[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].[C:13](=[O:16])([O-])[O-:14].[K+].[K+].C(O[C:24](=O)[N:25]([CH2:27][C:28]1[CH:29]=[C:30]([C:34]2[CH:39]=[CH:38][C:37]([OH:40])=[CH:36][CH:35]=2)[CH:31]=[CH:32][CH:33]=1)C)(C)(C)C>CC(N(C)C)=O.O>[C:3]([O:14][C:13]([CH2:24][NH:25][CH2:27][C:28]1[CH:29]=[C:30]([C:34]2[CH:39]=[CH:38][C:37]([O:40][C:2]3[CH:12]=[CH:11][CH:10]=[CH:9][C:3]=3[C:4]([O:6][CH2:7][CH3:8])=[O:5])=[CH:36][CH:35]=2)[CH:31]=[CH:32][CH:33]=1)=[O:16])([CH3:9])([CH3:4])[CH3:2]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 67953Benzoic acid, 2-fluoro-, ethyl esterHCID 69643261Tert-butyl(4'-hydroxybiphenyl-3-ylmethyl)methylcarbamate

생성물 1

HCID 21911050HCID 21911050, 화합물수율 104.9%

시약·촉매·용매 2

HCID 962Water용매HCID 31374Dimethylacetamide용매

실험 절차

2.15 g (12.8 mmol) of ethyl 2-fluorobenzoate and 1.9 g (14 mmol) of potassium carbonate are successively added to a solution of 4 g (12.8 mmol) of tert-butyl(4′-hydroxybiphenyl-3-ylmethyl)methylcarbamate in 45 ml of dimethylacetamide. The reaction medium is refluxed for 48 hours, cooled, diluted with water and extracted with ethyl acetate. The organic phase is dried over sodium sulfate, filtered and concentrated under vacuum. The residue obtained is purified by chromatography on a column of silica eluted with an 80/20 heptane/ethyl acetate mixture. 3.1 g of ethyl 2-{3′-[(tert-butoxycarbonylmethylamino)methyl]biphenyl-4-yloxy}benzoate are obtained in the form of a colorless oil, in a yield of 53%.

후처리

  1. temperatureThe reaction medium is refluxed for 48 hours
  2. temperaturecooled
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. customThe residue obtained
  8. customis purified by chromatography on a column of silica
  9. washeluted with an 80/20 heptane/ethyl acetate mixture

출처 및 근거

ORD 기록
ord-26c73ab41c454dd1858f0eff7961aaa0
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07125869B2

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