Methanol → HCID 68869975, Verbindung

HRID 1985273Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1985273
[C:1]([C:5]1[CH:35]=[CH:34][C:8]([CH2:9][N:10]2[CH2:14][CH:13]([CH2:15][CH2:16][CH2:17][C:18]3[CH:30]=[CH:29][C:21]([O:22][C:23]([CH3:28])([CH3:27])[C:24]([OH:26])=[O:25])=[C:20]([CH3:31])[CH:19]=3)[N:12]([CH3:32])[C:11]2=[O:33])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:36]O>S(=O)(=O)(O)O>[CH3:36][O:25][C:24](=[O:26])[C:23]([O:22][C:21]1[CH:29]=[CH:30][C:18]([CH2:17][CH2:16][CH2:15][CH:13]2[CH2:14][N:10]([CH2:9][C:8]3[CH:34]=[CH:35][C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])=[CH:6][CH:7]=3)[C:11](=[O:33])[N:12]2[CH3:32])=[CH:19][C:20]=1[CH3:31])([CH3:27])[CH3:28]

Komponenten

4

Edukt 2

HCID 887MethanolHCID 10195632HCID 10195632, Verbindung

Produkt 1

HCID 68869975HCID 68869975, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidKatalysator

Versuchsvorschrift

To a solution of 2-(4-{3-[1-(4-tert-Butyl-benzyl)-3-methyl-2-oxo-imidazolidin-4-yl]-propyl}-2-methyl-phenoxy)-2-methyl-propionic acid (0.610 g, 1.27 mmole) in methanol (10 mL) was added 15 drops of concentrated sulfuric acid. The mixture was stirred at room temperature overnight. After evaporated the solvent, the residue was partitioned between ethyl acetate (50 mL) and water (50 mL). The organic layer was washed by saturated sodium bicarbonate (50 mL), then brine (3×50 mL), dried over Na2SO4, filtered and concentrated in vacuo to produce an oil (0.624 g, 99%). Mass [EI+] 495 (M+H)+.

Aufarbeitung

  1. customAfter evaporated the solvent
  2. customthe residue was partitioned between ethyl acetate (50 mL) and water (50 mL)
  3. washThe organic layer was washed by saturated sodium bicarbonate (50 mL)
  4. dry with materialbrine (3×50 mL), dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2f91848927b448c1b084eb0b03b2558e
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07544812B2

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