Sodium Iodide → Rac-2-(methylamino)-1-pyrimidin-2-ylethanol
Reaktionsgleichung
Cl[CH2:2][CH:3]([C:5]1[N:10]=[CH:9][CH:8]=[CH:7][N:6]=1)[OH:4].[I-].[Na+].[CH3:13][NH2:14]>CO>[CH3:13][NH:14][CH2:2][CH:3]([C:5]1[N:10]=[CH:9][CH:8]=[CH:7][N:6]=1)[OH:4]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
In a pressure bottle was placed 2-chloro-1-pyrimidin-2-ylethanol (3.525 g, 22.24 mmol), sodium iodide (0.344 g, 2.29 mmol) and a 2M. methylamine solution (160 ml, 320 mmol) in methanol. The bottle was sealed and heated at 62° for 17 hr. The solvent was evaporated and the residue stirred with 10% MeOH—CHCl3. Filtration and evaporation gave a dark oil that was chromatographed over silica gel (90 g) eluting with 5-10% MeOH—CH2Cl2 containing 1% triethylamine The product was obtained as an amber oil (1.625 g).
Aufarbeitung
- customThe bottle was sealed
- temperatureheated at 62° for 17 hr
- customThe solvent was evaporated
- filtrationFiltration and evaporation
- customgave a dark oil that
- customwas chromatographed over silica gel (90 g)
- washeluting with 5-10% MeOH—CH2Cl2 containing 1% triethylamine The product
Quellen und Nachweise
- ORD-Eintrag
- ord-72ada895540946588e579aecb918c7bd
- Quelldatensatz
- uspto-grants-2005_03
- Patentnummer
- US06861438B2
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