反应详情

Lithium iodide dihydrate (25.5 g, 0.168 mole) in collidine (50 ml) under nitrogen were stirred and refluxed until the LiI dissolved. The amido-ester of Example 52 (17 g, 0.053 mole) in warm collidine (400 ml) was added and the solution stirred and refluxed for 48 hours. The cooled solution was poured into a mixture of 5N. HCl (800 ml., 4 mole) and ice, extracted with chloroform, which was washed with saturated sodium hydrogen carbonate solution, dried (NA2SO4), and evaporated to leave a semisolid. This was heated in vacuo with water to remove residual collidine, stirred with saturated sodium hydrogen carbonate solution, the solid filtered, washed with water and dried to give the title compound (7.85 g) (m.p. 202°-203° C.).

1. dissolutiondissolved
2. temperaturerefluxed for 48 hours
3. additionThe cooled solution was poured into a mixture of 5N
4. washwas washed with saturated sodium hydrogen carbonate solution
5. customdried (NA2SO4)
6. customevaporated
7. customto leave a semisolid
8. customto remove residual collidine
9. stirringstirred with saturated sodium hydrogen carbonate solution
10. filtrationthe solid filtered
11. washwashed with water
12. customdried