Reaktion #9825

Reaktionsgleichung

dimethylamine

tosylate

3-(2-bromo-phenyl)-3,4-dihydro-7-[2-(p-toluenesulfonyl)oxymethyl-benzodioxane-6-yl]amino-1-methyl-pyrimido[4,5-d]pyrimidin-2(1H)-one

→

3-(2-bromo-phenyl)-7-(2-dimethylaminomethyl-2,3-dihydro-benzo[1,4]dioxin-6-ylamino)-1-methyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one

Lösungsmittel

NMP

THF

NMP

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated to 50° C. for 4 hrs
2. 2
   workup.WAITto 65° C. for another 2 hrs
3. 3
   workup.STIRRINGStirring
4. 4
   workup.WAITwas continued at 45° C. over night
5. 5
   SonstigeSeparation by HPLC-MS
6. 6
   Sonstigeyielded crude product
7. 7
   Sonstigewas further purified
8. 8
   workup.DISSOLUTIONby dissolving in CHCl3
9. 9
   Waschenwashing with water

Vorschrift

90 mg of the tosylate from example 4 in 8 ml NMP were treated with 0.62 ml 2 M dimethylamine in THF and stirred at room temperature for 3 d. The mixture was heated to 50° C. for 4 hrs, then to 65° C. for another 2 hrs. Stirring was continued at 45° C. over night. Separation by HPLC-MS yielded crude product contaminated by NMP, which was further purified by dissolving in CHCl3 and washing with water.

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