反应详情

The product from Example 15B (950 mg, 5.37 mmol) was dissolved in CH2Cl2 (20 mL). Triethylamine (1.10 mL, 7.89 mmol) and m-toluidine (0.70 mL, 6.46 mmol) were added, and the reaction stirred at ambient temperature for 2 h. The reaction mixture was diluted with 0.1M HCl (100 mL) and extracted with CH2Cl2 (3×50 mL). The organic extracts were combined, washed with brine (50 mL), dried over MgSO4, filtered and concentrated under vacuum. The residue was purified by silica gel chromatography (2.5% EtOAc in CH2Cl2, Rf=0.39) to afford the title compound as a white solid (1.11 g, 83%). MS (DCI/NH3) m/z 248 (M+H)+.

1. extractionextracted with CH2Cl2 (3×50 mL)
2. washwashed with brine (50 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customThe residue was purified by silica gel chromatography (2.5% EtOAc in CH2Cl2, Rf=0.39)