反应详情

To 10 g. (0.044 moles) of 4-amino-2-(methylphenylamino)-5-pyrimidine-carbonitrile in 200 ml. of tetrahydrofuran was added 6.7 g. (0.044 moles) of ethyl malonyl chloride and then this mixture was heated at reflux for 2 hours. The reaction was then filtered and the filtercake rinsed with tetrahydrofuran. The filtrate was evaporated to dryness on a rotary evaporator. The viscous liquid residue was treated with 50 ml. of 20% NaOH and heated to boiling for 5 minutes. The resulting solid was removed by filtration. This solid was slurried in water, acidified with acetic acid and filtered. The crude product was recrystallized from 95% ethanol to give 1.05 g. of solid with m.p. 297° C. (dec.).

1. temperatureat reflux for 2 hours
2. filtrationThe reaction was then filtered
3. washthe filtercake rinsed with tetrahydrofuran
4. customThe filtrate was evaporated to dryness on a rotary evaporator
5. additionThe viscous liquid residue was treated with 50 ml
6. temperatureof 20% NaOH and heated
7. customThe resulting solid was removed by filtration
8. filtrationfiltered
9. customThe crude product was recrystallized from 95% ethanol
10. customto give 1.05 g