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Hydrochloric Acid → 3-(2-Fluoro-4-{[4-({[2-(4-fluorophenyl)ethyl][4-(4-fluorophenyl)-1,3-thiazol-2-yl]amino}methyl)benzyl]oxy}-phenyl)propanoic acid

HRID 732225
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HRID 732225 반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=1)=O.[F:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][CH2:20][NH:21][C:22]([NH2:24])=[S:23])=[CH:15][CH:14]=1.[H-].[Na+].Cl[CH2:28][C:29]1[CH:50]=[CH:49][C:32]([CH2:33][O:34][C:35]2[CH:40]=[CH:39][C:38]([CH2:41][CH2:42][C:43]([O:45]CC)=[O:44])=[C:37]([F:48])[CH:36]=2)=[CH:31][CH:30]=1.Cl>C(O)C.O1CCCC1.[OH-].[Na+].CN(C)C=O>[F:48][C:37]1[CH:36]=[C:35]([O:34][CH2:33][C:32]2[CH:49]=[CH:50][C:29]([CH2:28][N:21]([CH2:20][CH2:19][C:16]3[CH:15]=[CH:14][C:13]([F:12])=[CH:18][CH:17]=3)[C:22]3[S:23][CH:2]=[C:3]([C:5]4[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=4)[N:24]=3)=[CH:30][CH:31]=2)[CH:40]=[CH:39][C:38]=1[CH2:41][CH2:42][C:43]([OH:45])=[O:44]
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참가 물질

10

반응물 5

HCID 313Hydrochloric Acid2회HCID 24758Sodium hydrideHCID 967492-Bromo-1-(4-fluorophenyl)ethan-1-oneHCID 23143241Ethyl 3-(4-([4-(chloromethyl)benzyl]oxy}-2-fluorophenyl)propanoateHCID 23143277N-[2-(4-fluorophenyl)ethyl]thiourea

생성물 1

HCID 23143329
3-(2-Fluoro-4-{[4-({[2-(4-fluorophenyl)ethyl][4-(4-fluorophenyl)-1,3-thiazol-2-yl]amino}methyl)benzyl]oxy}-phenyl)propanoic acid
수율 44%

시약·촉매·용매 4

HCID 702Ethanol용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매HCID 14798Sodium Hydroxide용매

실험 절차

A mixture of 2-bromo-1-(4-fluorophenyl)ethanone (217 mg, 1.0 mmol), N-[2-(4-fluorophenyl)ethyl]thiourea (198 mg, 1.0 mmol) and N,N-dimethylformamide (5 mL) was stirred at room temperature for 1 hr. Sodium hydride (100 mg, in oil, 2.5 mmol) was added to the reaction mixture at room temperature, and the mixture was stirred at room temperature for 1 hr. Ethyl 3-(4-{[4-(chloromethyl)benzyl]oxy}-2-fluorophenyl)propanoate (350 mg, 1.0 mmol) was added, and the mixture was further stirred at room temperature for 2 hr. The reaction mixture was poured into 1N hydrochloric acid and the mixture was extracted with ethyl acetate. The organic layer was concentrated. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:19-3:2 in volume ratio) to give a yellow oil. The oil was dissolved in a mixed solvent of ethanol (5 mL) and tetrahydrofuran (5 mL), and 2N aqueous sodium hydroxide solution (2 mL) was added. The mixture was stirred at room temperature for 2 hr. The reaction mixture was poured into 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and concentrated to give the title compound (264 mg, yield 44%, 3 steps) as a pale-green oil.

후처리

  1. stirringthe mixture was stirred at room temperature for 1 hr
  2. stirringthe mixture was further stirred at room temperature for 2 hr
  3. extractionthe mixture was extracted with ethyl acetate
  4. concentrationThe organic layer was concentrated
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:19-3:2 in volume ratio)
  6. customto give a yellow oil
  7. additionwas added
  8. stirringThe mixture was stirred at room temperature for 2 hr
  9. extractionthe mixture was extracted with ethyl acetate
  10. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-674d648921d6448792b665071b3a4598
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07585880B2

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