反应详情

A solution of ethyl 2-mercaptoacetate (1.47 mL) in DMF (48 mL) was ice-cooled and treated with sodium hydride (540 mg of a 60% dispersion in oil). After 1 h methyl 6-amino-5-bromopyridine-2-carboxylate (3 g) (T. R. Kelly and F. Lang, J. Org. Chem. 61, 1996, 4623-4633) was added and the mixture stirred for 16 h at room temperature. The solution was diluted with EtOAc (1 L), washed with water (3×300 mL), dried and evaporated to about 10 mL. The white solid was filtered off and washed with a little EtOAc to give the ester (0.95 g); LC/MS (APCI−) m/z 223 ([M−H]−, 100%).

1. temperaturecooled
2. addition61, 1996, 4623-4633) was added
3. washwashed with water (3×300 mL)
4. customdried
5. customevaporated to about 10 mL
6. filtrationThe white solid was filtered off
7. washwashed with a little EtOAc