反应详情

2,6-dichloropyrazine (1.02 g, 6.85 mmol) was dissolved in DMSO (7 mL). The product from Example 1C (1.61 g, 7.58 mmol) and N,N-diisopropylethylamine (1.5 mL, 8.61 mmol) were added to the reaction mixture. The reaction was stirred at ambient temperature for 23 h. The reaction was diluted with water (200 mL) and extracted with CH2Cl2 (4×100 mL). The organic extracts were combined and washed with and brine (150 mL), dried over MgSO4, filtered and concentrated under vacuum. The residue was purified by silica gel chromatography (EtOAc, Rf=0.38) to afford the title compound as a white solid (1.99 g, 89%). MS (DCI/NH3) m/z 325 (M+H)+.

1. extractionextracted with CH2Cl2 (4×100 mL)
2. washwashed with and brine (150 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customThe residue was purified by silica gel chromatography (EtOAc, Rf=0.38)