Reaktion #1781912

Reaktionsgleichung

citric acid

Sodium hydride

2-methyl-1,2,5-thiadiazolidine 1,1-dioxide

product

2,5-Dibromo-4-methyl-pyrimidine

→

5-Bromo-4-methyl-2-(5-methyl-1,1-dioxido-1,2,5-thiadiazolidin-2-yl)-pyrimidine

Lösungsmittel

THF

DMF

water

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated at 60° C. for 10 min
2. 2
   Extraktionextracted with ethylacetate
3. 3
   SonstigeThe organics were evaporated under reduced pressure
4. 4
   Sonstigethe residue purified by chromatography on silica eluting with diethylether, yield 0.58 g

Vorschrift

Sodium hydride (0.128 g, 60% disp. in oil) was added to a stirred solution of 2-methyl-1,2,5-thiadiazolidine 1,1-dioxide (0.433 g) in THF (10 ml). DMF (10 ml) was added and the mixture heated at 80° C. for 5 min then a solution of the product from step (i) (0.8 g) in DMF (5 ml) was added. The mixture was heated at 60° C. for 10 min, poured into water (100 ml), acidified with citric acid and extracted with ethylacetate. The organics were evaporated under reduced pressure and the residue purified by chromatography on silica eluting with diethylether, yield 0.58 g.

Quelle