反应详情

The cyclization was effected by heating 12.3 g (0.037 mole) of N-[3-[[(4-chloro-2-pyridinyl)carbonyl]amino]-2-pyridinyl]glycine ethyl ester at 200°-210° C. (oil bath) for 15 minutes. The dark residue was dissolved in methylene chloride and filtered. The filtrate was treated with Florisil®, filtered, and evaporated to an oil, which crystallized upon standing. The solid was recrystallized from methanol-water, washed with 50% aqueous methanol, and dried under high vacuum at 50° C. overnight to give 2.44 g (21%) of title compound, mp 99°-101° C.

1. filtrationfiltered
2. additionThe filtrate was treated with Florisil®
3. filtrationfiltered
4. customevaporated to an oil, which
5. customcrystallized
6. customThe solid was recrystallized from methanol-water
7. washwashed with 50% aqueous methanol
8. customdried under high vacuum at 50° C. overnight