反应详情

A 5 L round-bottom flask was charged with methanol (100 mL), the ketoamide 2-3 (200 g), and ammonium acetate (110.4 g). Methanol (180 mL) and 28% aqueous ammonium hydroxide (58.6 mL) were then added keeping the temperature below 30° C. during the addition. Additional methanol (100 mL) was added to the reaction mixture. The mixture was heated at reflux temperature and aged for 2 h. The reaction was cooled to room temperature and then to about 5° C. in an ice-bath. After 30 min, the solid was filtered and dried to afford 2-4 as a solid (180 g); m.p. 271.2° C.

1. customthe temperature below 30° C.
2. additionduring the addition
3. temperatureThe mixture was heated
4. temperatureat reflux temperature
5. customto about 5° C.
6. waitAfter 30 min
7. filtrationthe solid was filtered
8. customdried