反应详情

温度

-20 °C

To 1.5 g (7.3 mM) of 4-chloro-6-phenyl-2-pyrimidinamine is added 40 ml of glacial acetic acid and 1.05 g of N-chlorosuccinimide. The reaction is stirred at ambient temperature (-20° C.) for 18 hours. The reaction mixture is evaporated to dryness, dissolved in acetone and 10.0 g of silica gel added and the mixture evaporated to a powder under vacuum. The powder is chromatographed on 50 g silica gel and eluted with 35% ethyl acetate/hexane. A fraction containing material with a TLC r.f. of 0.7 35% ethylacetate/hexane is collected and evaporated to dryness, recrystallized from acetone/Skellysolve B (1:10), evaporated to dryness(?) to yield 0.90 g of 4,5-dichloro-6-phenyl-2-pyrimidinamine.

1. customThe reaction mixture is evaporated to dryness
2. dissolutiondissolved in acetone
3. addition10.0 g of silica gel added
4. customthe mixture evaporated to a powder under vacuum
5. customThe powder is chromatographed on 50 g silica gel
6. washeluted with 35% ethyl acetate/hexane
7. additionA fraction containing material with a TLC r.f
8. customof 0.7 35% ethylacetate/hexane is collected
9. customevaporated to dryness
10. customrecrystallized from acetone/Skellysolve B (1:10)
11. customevaporated