Reaktion #3505

Reaktionsgleichung

2,7-diamino-6-o-tolyl-pyrido[2,3-d]pyrimidine

sodium hydride

t-butylisocyanate

→

title compound

1-tert-Butyl-3-[7-(3-tert-butylureido)-6-o-tolyl-pyrido[2,3-d]pyrimidin-2-yl]urea

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprepared
2. 2
   workup.STIRRINGthe mixture stirred overnight at ambient temperature
3. 3
   FiltrationThe reaction mixture is filtered
4. 4
   Sonstigeto remove insoluble salts
5. 5
   Sonstigethe filtrate evaporated under reduced pressure
6. 6
   workup.ADDITIONThe residue is diluted with water
7. 7
   Filtrationthe insoluble crude product collected by filtration
8. 8
   Sonstigedried in vacuo
9. 9
   SonstigeCrystallization from a hexane

Vorschrift

A suspension of 0.5 g of 2,7-diamino-6-o-tolyl-pyrido[2,3-d]pyrimidine, prepared as described above in Example 1, in 10 mL of dimethylformamide is reacted with 0.16 g of 60% sodium hydride and stirred at ambient temperature for 1.5 hours. To the suspension is added 0.49 mL of t-butylisocyanate and the mixture stirred overnight at ambient temperature. The reaction mixture is filtered to remove insoluble salts and the filtrate evaporated under reduced pressure. The residue is diluted with water, the insoluble crude product collected by filtration and dried in vacuo. Crystallization from a hexane:ethyl acetate: dichloromethane mixture (3:2:5 v/v/v) afforded the title compound, mp 209°-212° C. dec.

Quelle