Reaktion #91961

Reaktionsgleichung

NH4Cl

5-methyloxazole-4-carbonitrile

MeONa

→

5-methyloxazole-4-carboxamidine

Lösungsmittel

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 2 h
2. 2
   SonstigeThe solvent was removed
3. 3
   Sonstigethe residue was purified by flash chromatography (Biotage, 40 g silica gel, MeOH in DCM 5%˜35%)
4. 4
   Sonstigeto afford brown solid AB (587 mg, 67%)

Vorschrift

To a solution of 5-methyloxazole-4-carbonitrile AA (0.76 g, 7.0 mmol) in anhydrous MeOH (30 mL) was added MeONa (0.57 g, 10 mmol), after stirred at 35° C. under nitrogen for 3 h, NH4Cl (0.75 g, 14 mmol) was added, refluxed for 2 h. The solvent was removed and the residue was purified by flash chromatography (Biotage, 40 g silica gel, MeOH in DCM 5%˜35%) to afford brown solid AB (587 mg, 67%). 1H NMR (DMSO-d6, 400 MHz) δ ppm: 9.11-9.19 (m, 3H), 8.60 (s, 1H), 2.59 (s, 3H). MS: calc'd (MH+) 126, measured (MH+) 126.

Quelle