反应详情

The product of Example 12 (1.00 g, 2.32 mmol) was added to 5 ml of 40% aqueous methylamine in dimethylformamide (3-5 mL) and the mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with water and extracted with ethyl acetate (3x). The combined organic extracts were washed with water, brine, dried (MgSO4) and concentrated in vacuo. The crude residue (0.54 g) was purified by chromatography (Silica Gel 60, first with 2% methanol in methylene chloride and then with 50% ethyl acetate in hexanes) to give 300 mg (37.5%) of pure title compound as a yellow solid, mp 126.5°-127° C. (ethanol).

1. extractionextracted with ethyl acetate (3x)
2. washThe combined organic extracts were washed with water, brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe crude residue (0.54 g) was purified by chromatography (Silica Gel 60