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Diisopropylamine → Ethyl 3-hydroxy-3-(1-trityl-1h-imidazol-4-yl)propanoate

HRID 724205
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 724205
C(NC(C)C)(C)C.C([Li])CCC.[C:13]([N:32]1[CH:36]=[C:35]([CH:37]=[O:38])[N:34]=[CH:33]1)([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[Cl-].[NH4+].[C:41]([O:44][CH2:45][CH3:46])(=[O:43])[CH3:42]>C1COCC1.CCCCCC.O>[OH:38][CH:37]([C:35]1[N:34]=[CH:33][N:32]([C:13]([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:36]=1)[CH2:42][C:41]([O:44][CH2:45][CH3:46])=[O:43]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 7912DiisopropylamineHCID 8857Ethyl AcetateHCID 25517Ammonium ChlorideHCID 6182331-(triphenylmethyl)-1H-imidazole-4-carbaldehydeHCID 178418339Butyllithium

Produkt 1

HCID 21879633Ethyl 3-hydroxy-3-(1-trityl-1h-imidazol-4-yl)propanoate

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel3×HCID 8058HexaneLösungsmittel

Reaktionsbedingungen

Temperatur
-70 °C

Versuchsvorschrift

Diisopropylamine (33.8 ml) was dissolved in dry THF (445 ml) under an argon atmosphere. A solution (1.6 M; 150 ml) of n-butyl lithium in hexane was added at not more than 0° C. with stirring under ice-cooling (ice-salt), and the mixture was stirred for 30 min. The mixture was then cooled to −70° C. in a dry ice-acetone bath and ethyl acetate (23.5 ml)/dry THF (60 ml) solution was added at not more than −65° C. The mixture was stood with stirring for 1 h 20 min. The reaction mixture was added to a solution (1185 ml) cooled to −70° C. of 1-trityl-4-formyl-1H-imidazole (67.7 g) in dry THF at not more than −60° C., and the mixture was stirred for 1 h. A 20% aqueous ammonium chloride solution (445 ml) was added to stop the reaction and the mixture was allowed to warm to room temperature over 1 h. An equivalent amount of water was added and the mixture was partitioned. The aqueous layer was extracted with ethyl acetate. The organic layer was combined and the mixture was dried over anhydrous sodium sulfate. The solvent was evaporated, and the precipitated crystals were finely divided with hexane, collected by filtration and dried to give the title compound (77.26 g) as colorless crystals.

Aufarbeitung

  1. stirringthe mixture was stirred for 30 min
  2. stirringwith stirring for 1 h 20 min
  3. stirringthe mixture was stirred for 1 h
  4. customthe reaction
  5. temperatureto warm to room temperature over 1 h
  6. customthe mixture was partitioned
  7. extractionThe aqueous layer was extracted with ethyl acetate
  8. dry with materialthe mixture was dried over anhydrous sodium sulfate
  9. customThe solvent was evaporated
  10. filtrationcollected by filtration
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e8f2cfee87f549c2adf8dd519bd6cbd0
Quelldatensatz
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07141598B2

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