반응 #42049

반응 방정식

2-[(6-chloro)pyrimidin-4-ylamino]-1-methyl-4-nitrobenzene

dihydroxy(5-pyrimidinyl)borane

→

objective compound

수율 21.1%

1-methyl-4-nitro-2-[6-(5-pyrimidinyl)pyrimidin-4-ylamino]benzene

수율 21.1%

용매

ethanol

반응 조건

후처리

1. 1
   기타by purging with argon
2. 2
   workup.ADDITION5.82 g of potassium carbonate and 2.15 g of tetrakis(triphenylphosphine)palladium (0) were added in turn
3. 3
   온도the mixture was heated
4. 4
   온도at reflux for 7.5 hours
5. 5
   workup.ADDITIONThe reaction solution was mixed with water
6. 6
   추출followed by extraction with ethyl acetate twice
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
9. 9
   기타The residue was crystallized
10. 10
    workup.ADDITIONby adding chloroform-methanol

실험 절차

3.28 g of 2-[(6-chloro)pyrimidin-4-ylamino]-1-methyl-4-nitrobenzene (Reference Example 20 (step 1)) were dissolved with heating in 130 ml of anhydrous ethanol. 1.69 g of dihydroxy(5-pyrimidinyl)borane was added, and then deaeration was performed, followed by purging with argon. 5.82 g of potassium carbonate and 2.15 g of tetrakis(triphenylphosphine)palladium (0) were added in turn, and then the mixture was heated at reflux for 7.5 hours. The reaction solution was mixed with water, followed by extraction with ethyl acetate twice, and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was crystallized by adding chloroform-methanol to obtain 808 mg of the objective compound as ocherous crystals.

출처