反应详情

A solution of 3-amino-6-bromo-pyrazine-2-carboxylic acid (0.62 g, 2.8 mmol), HATU (1.3 g, 3.4 mmol) and di-isopropylethylamine (1.72 ml, 3.5 mmol) in DMF (20 ml) is stirred at room temperature for 5 minutes. N-Methoxy-N-methylamine hydrochloride (0.33 g, 3.4 mmol) is added and the reaction is stirred at room temperature for 2 hours. The solvent is concentrated in vacuo and the residue dissolved in EtOAc (30 ml), and washed with sat. aq. NaHCO3 (20 ml), 0.1N HCl (20 ml), dried (MgSO4) and concentrated in vacuo to yield a brown oil. Purification by flash chromatography (SiO2, 30% EtOAc in iso-hexane) yields 3-amino-6-bromo-pyrazine-2-carboxylic acid methoxy-methyl-amide as a yellow solid [M+H]+261.

1. concentrationThe solvent is concentrated in vacuo
2. dissolutionthe residue dissolved in EtOAc (30 ml)
3. washwashed with sat. aq. NaHCO3 (20 ml), 0.1N HCl (20 ml)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto yield a brown oil
7. customPurification by flash chromatography (SiO2, 30% EtOAc in iso-hexane)