反应详情

A solution of 9 (1.00 g) in DME/NH3 (50 ml) was heated at 80° C. in a steel bomb for 24 hours. After cooling, the solvent was evaporated and the solid obtained was stirred in NH3 /MeOH (100 ml) overnight. After the evaporation of the solvent, the residue was dissolved in water (50 ml), washed with CHCl3 (2×25 ml) and ether (2×25 ml). The water layer was evaporated and the residue crystallized from water to give pure 10 (0.30 g, 67%) as white crystals: m.p. 225° C. (dec).

1. temperatureAfter cooling
2. customthe solvent was evaporated
3. customthe solid obtained
4. customAfter the evaporation of the solvent
5. dissolutionthe residue was dissolved in water (50 ml)
6. washwashed with CHCl3 (2×25 ml) and ether (2×25 ml)
7. customThe water layer was evaporated
8. customthe residue crystallized from water