Acetone → 5-Pyrimidinol, hexahydro-2,2-dimethyl-5-phenyl-

HRID 623203Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 623203
Cl.Cl.[OH:3][C:4]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([CH2:7][NH2:8])[CH2:5][NH2:6].[OH-].[Na+].[CH3:17][C:18]([CH3:20])=O>O>[CH3:17][C:18]1([CH3:20])[NH:8][CH2:7][C:4]([OH:3])([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:5][NH:6]1

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 14798Sodium HydroxideHCID 21290601HCID 21290601, Verbindung

Produkt 1

HCID 30874705-Pyrimidinol, hexahydro-2,2-dimethyl-5-phenyl-Ausbeute 68,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

4.4 g (0.01841 mol) of the dihydrochloride obtained in stage (c) above are dissolved in 50 ml of water. 2.2 g of sodium hydroxide pellets and 3 ml of acetone are added. The mixture is left to stand overnight at room temperature (15°-20° C.) and extracted with 3×100 ml of CHCl3, and the chloroform phase is washed with 30 ml of water, dried over MgSO4 and then filtered to remove MgSO4. The filtrate is evaporated to dryness; recrystallization from petroleum ether (fraction boiling at 45°-60° C.) gives 2.6 g (yield: 68.5%) of CRL 41 365. M.p.=108° C.

Aufarbeitung

  1. waitThe mixture is left
  2. extraction(15°-20° C.) and extracted with 3×100 ml of CHCl3
  3. washthe chloroform phase is washed with 30 ml of water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customto remove MgSO4
  7. customThe filtrate is evaporated to dryness
  8. customrecrystallization from petroleum ether (fraction boiling at 45°-60° C.)
  9. customgives 2.6 g (yield: 68.5%) of CRL 41 365

Quellen und Nachweise

ORD-Eintrag
ord-3a4322d0a09041559f0772612c7e895d
Quelldatensatz
uspto-grants-1988_09
Patentnummer
US04774248

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