Sodium ethoxide → HCID 67299931, Verbindung

Temperatur

50 °C

To a solution of 2-methoxy-acetamidine (7.21 g, 89.19 mmol) in EtOH (50 ml) was added sodium ethylate (26 ml, 22% solution in EtOH) and the reaction mixture was heated to 50° C. for 30 min. A solution of mucobromic acid (6.5 g, 38.77 mmol) in EtOH (50 ml) was added followed by sodium ethylate (14 ml, 22% solution in EtOH), and the reaction mixture was continued to stir at 50° C. for 1 h. After filtration and solvent evaporation, water (5 ml) was added, the reaction mixture was cooled to 0° C. and acidified with 2N HCl solution to pH ˜6. After evaporation of water, the residue was dissolved in MeOH, filtered, and the filtrate was evaporated. The crude material was purified by silica gel chromatography using a methanol/methylenechloride eluent as solvent to yield 3.73 g (60%) of the title compound.

1. filtrationAfter filtration and solvent evaporation, water (5 ml)
2. additionwas added
3. temperaturethe reaction mixture was cooled to 0° C.
4. customAfter evaporation of water
5. dissolutionthe residue was dissolved in MeOH
6. filtrationfiltered
7. customthe filtrate was evaporated
8. customThe crude material was purified by silica gel chromatography

ORD-Eintrag

ord-be05cd47755949cbba5342027fb8131f

Quelldatensatz

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08470820B2