反应详情

The product of step v) (0.2 g) and diethoxymethyl acetate (10 ml) were stirred at ambient temperature under nitrogen for 1 hour, then at 80° for 24 hours. Evaporation afforded a residue which was treated with liquid ammonia (15 ml) in an autoclave at 60° for 16 hours. The ammonia was allowed to evaporate and the residue taken up in 0.5M hydrochloric acid (10 ml) at 60° for 45 min. The volatiles were removed in vacuo and the remaining material dissolved in water (10 ml). Upon neutralisation with concentrated ammonia the sub-title compound crystallised and was collected and dried (0.15 g).

1. customEvaporation
2. customafforded a residue which
3. customto evaporate
4. waitthe residue taken up in 0.5M hydrochloric acid (10 ml) at 60° for 45 min
5. customThe volatiles were removed in vacuo
6. dissolutionthe remaining material dissolved in water (10 ml)
7. customUpon neutralisation with concentrated ammonia the sub-title compound crystallised
8. customwas collected
9. customdried (0.15 g)