StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

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
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 732225
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]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 5

HCID 313Hydrochloric Acid2×HCID 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

Produkt 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
Ausbeute 44 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 702EthanolLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-674d648921d6448792b665071b3a4598
Quelldatensatz
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07585880B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion