反应详情

The product from Step 1 (21.17 g, 51 mmol) was dissolved in ammonia, 2M in methanol (400 mL, 800 mmol) that was further saturated with anhydrous ammonia. The solution was heated to reflux for 16 hr overnight, and allowed to cool to room temperature. The solution was concentrated and the residue was dissolved in ethyl acetate and water. The ethyl acetate layer was washed twice with water, dried with brine, and concentrated to give a yellow solid. The solid was recrystallized from ethyl acetate/hexane to give a white powder that was washed with hexane and air dried (9.65 g, 56.8%).

1. temperatureThe solution was heated
2. temperatureto reflux for 16 hr overnight
3. concentrationThe solution was concentrated
4. dissolutionthe residue was dissolved in ethyl acetate
5. washThe ethyl acetate layer was washed twice with water
6. dry with materialdried with brine
7. concentrationconcentrated
8. customto give a yellow solid
9. customThe solid was recrystallized from ethyl acetate/hexane
10. customto give a white powder that
11. washwas washed with hexane and air
12. customdried (9.65 g, 56.8%)