HCID 57718998, Verbindung → HCID 10195632, Verbindung

HRID 1985123Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1985123
C([O:3][C:4](=[O:37])[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH2:17][CH:18]2[CH2:22][N:21]([CH2:23][C:24]3[CH:29]=[CH:28][C:27]([C:30]([CH3:33])([CH3:32])[CH3:31])=[CH:26][CH:25]=3)[C:20](=[O:34])[N:19]2[CH3:35])=[CH:11][C:10]=1[CH3:36])([CH3:7])[CH3:6])C>CO>[C:30]([C:27]1[CH:28]=[CH:29][C:24]([CH2:23][N:21]2[CH2:22][CH:18]([CH2:17][CH2:16][CH2:15][C:12]3[CH:13]=[CH:14][C:9]([O:8][C:5]([CH3:6])([CH3:7])[C:4]([OH:37])=[O:3])=[C:10]([CH3:36])[CH:11]=3)[N:19]([CH3:35])[C:20]2=[O:34])=[CH:25][CH:26]=1)([CH3:31])([CH3:32])[CH3:33]

Komponenten

3

Edukt 1

HCID 57718998HCID 57718998, Verbindung

Produkt 1

HCID 10195632HCID 10195632, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

2-(4-{3-[1-(4-tert-Butyl-benzyl)-3-methyl-2-oxo-imidazolidin-4-yl]-propyl}-2-methyl-phenoxy)-2-methyl-propionic acid ethyl ester (0.065 g, 0.128 mmole) is treated with 3:1 MeOH/5.0N NaOH (4 mL) at room temperature overnight, and then concentrated. The resulting residue is diluted with water (2 mL), cooled down to 0° C., acidified to pH=2 by adding concentrated HCl dropwise. The aqueous suspension is loaded on a Chem elut tube and eluted with DCM (50 mL). Evaporation of methylene chloride gives the titled compound as an oil (0.060 g, 98%). Mass [EI+] 481 (M+H)+, [EI−] 479 (M−H)−.

Aufarbeitung

  1. concentrationconcentrated
  2. additionThe resulting residue is diluted with water (2 mL)
  3. additionby adding concentrated HCl dropwise
  4. washeluted with DCM (50 mL)
  5. customEvaporation of methylene chloride

Quellen und Nachweise

ORD-Eintrag
ord-16bc7c04ce9b40a4821aa1cb8ecb75d0
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07544812B2

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