Reaktion #1781911

Reaktionsgleichung

Isoamylnitrite

5-bromo-4-methyl-2-pyrimidinamine

bromoform

isohexane

→

2,5-Dibromo-4-methyl-pyrimidine

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   WaschenThe silica was washed with petrol (1000 ml), dichloromethane (200 ml)
3. 3
   Waschenthe product eluted with ethylacetate
4. 4
   SonstigeThe ethylacetate layer was evaporated under reduced pressure
5. 5
   Sonstigethe residue purified by chromatography on silica eluting with 5% diethylether/isohexane, yield 0.9 g

Vorschrift

Isoamylnitrite (21 ml) was added to a stirred suspension of 5-bromo-4-methyl-2-pyrimidinamine (1.75 g) in bromoform (30 ml) and the mixture heated at 85° C. for 4 h. After cooling, isohexane (300 ml) was added and the solution passed through a pad of silica-gel. The silica was washed with petrol (1000 ml), dichloromethane (200 ml) then the product eluted with ethylacetate. The ethylacetate layer was evaporated under reduced pressure and the residue purified by chromatography on silica eluting with 5% diethylether/isohexane, yield 0.9 g

Quelle