반응 #1869196

반응 방정식

ethyl 2-mercaptoacetate

sodium hydride

methyl 6-amino-5-bromopyridine-2-carboxylate

→

ester

Methyl 3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]thiazine-6-carboxylate

용매

DMF

EtOAc

반응 조건

후처리

1. 1
   온도cooled
2. 2
   workup.ADDITION61, 1996, 4623-4633) was added
3. 3
   세척washed with water (3×300 ml)
4. 4
   기타dried
5. 5
   기타evaporated to about 10 ml
6. 6
   여과The white solid was filtered off
7. 7
   세척washed with a little EtOAc

실험 절차

A solution of ethyl 2-mercaptoacetate (1.473 ml) in DMF (48 ml) was ice-cooled and treated with sodium hydride (540 mg of a 60% dispersion in oil). After 1 hour 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 hours at room temperature. The solution was diluted with EtOAc (1 litre), 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).

출처