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Toluene → 1-Adamantan-2-yl-3-benzyl-1,3-dihydro-imidazol-2-one

HRID 1092302
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1092302
C(OC(=O)C[N:6]([CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:7]([NH:9][CH:10]1[CH:17]2CC3CC(CC1C3)C2)=[O:8])C.[C:28]1([CH3:34])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[H-].[CH2:36]([Al+]CC(C)C)[CH:37](C)[CH3:38]>C(Cl)Cl>[CH:28]12[CH2:34][CH:37]3[CH2:38][CH:32]([CH2:31][CH:30]([CH2:36]3)[CH:29]1[N:9]1[CH:10]=[CH:17][N:6]([CH2:20][C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[C:7]1=[O:8])[CH2:33]2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1140TolueneHCID 21225700DiisobutylaluminumhydrideHCID 66593062HCID 66593062, Verbindung

Produkt 1

HCID 249640651-Adamantan-2-yl-3-benzyl-1,3-dihydro-imidazol-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

(3-Adamantan-2-yl-1-benzyl-ureido)-acetic acid ethyl ester (450 mg) was dissolved in dry DCM (5 mL) and toluene (5 mL) under argon and cooled to −78° C. Diisobutylaluminium hydride (1 M solution in DCM, 1.46 mL) was added drop by drop over 5 minutes and the mixture was allowed to stir at −78° C. for 30 minutes. The cooling bath was removed and after 10 minutes, the reaction mixture was quenched by addition of aqueous potassium sodium tartrate solution (1M, 15 mL). The mixture was extracted with chloroform twice and the combined organic extracts were washed with brine. The combined organic layers were shaken with 25% HCl (30 mL) for 5 minutes and the layers were separated. The organic solution was dried with sodium sulfate, filtered and evaporated to give a crude product that was purified by flash chromatography using a gradient of 20% to 80% ethyl acetate in heptane as an eluent. The fractions containing the product were combined and evaporated to give 1-adamantan-2-yl-3-benzyl-1,3-dihydro-imidazol-2-one as a white solid (276 mg). MS (EI): 308.2 (M+).

Aufarbeitung

  1. customThe cooling bath was removed and after 10 minutes
  2. customthe reaction mixture was quenched by addition of aqueous potassium sodium tartrate solution (1M, 15 mL)
  3. extractionThe mixture was extracted with chloroform twice
  4. washthe combined organic extracts were washed with brine
  5. stirringThe combined organic layers were shaken with 25% HCl (30 mL) for 5 minutes
  6. customthe layers were separated
  7. dry with materialThe organic solution was dried with sodium sulfate
  8. filtrationfiltered
  9. customevaporated
  10. customto give a crude product that
  11. customwas purified by flash chromatography
  12. additionThe fractions containing the product
  13. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-7ef8cde18e584b9fa484018d5945a601
Quelldatensatz
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08129423B2

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