反应详情

A mixture of N-[3-[(3,4-dichlorobenzoyl)amino]-2-pyridinyl]glycine ethyl ester (33 g, 0.09 mole) and 167 ml of ethylene glycol was heated at reflux for 11/2 hr. The material crystallized upon cooling. A small portion of the solid was collected by filtration, washed with water, and dried under high vacuum. The solid was recrystallized from ethanol with refrigeration, collected by filtration, washed with ethanol/water mixture, and dried under high vacuum at 70° C. over 2 days to give 2.0 g, mp 141°-42° C.

1. temperaturewas heated
2. temperatureat reflux for 11/2 hr
3. customThe material crystallized
4. temperatureupon cooling
5. filtrationA small portion of the solid was collected by filtration
6. washwashed with water
7. customdried under high vacuum
8. customThe solid was recrystallized from ethanol with refrigeration
9. filtrationcollected by filtration
10. washwashed with ethanol/water mixture
11. customdried under high vacuum at 70° C. over 2 days
12. customto give 2.0 g, mp 141°-42° C.