反应详情

A mixture of 43 mg of N-(4-amino-2-methyl-6-quinolyl)-2-amino-4,6-dichloro-5-methylsulfanylpyrimidine and 55 mg of 4,6-diamino-2-methylquinoline in 5 mL of ethanol is heated under reflux for about 3 hours, left at a temperature in the region of 20° C. for about 16 hours and then filtered. The filtrate is concentrated under reduced pressure (2.7 kPa) at a temperature in the region of 40° C., and then the residue obtained is purified by HPLC (column: C18 Waters, 5 M, 50×19 mm; eluent: elution gradient water-acetonitrile-TFA (0.07%) from 95-5 to 5-95 over 30 minutes). The fractions containing the desired product are combined and concentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the region of 40° C. to obtain 12 mg of N,N′-bis(4-amino-2-methyl-6-quinolyl)-2,4-diamino-6-chloro-5-methylsulfanyl-pyrimidine in the form of a beige colored solid.

1. temperatureis heated
2. temperatureunder reflux for about 3 hours
3. filtrationfiltered
4. concentrationThe filtrate is concentrated under reduced pressure (2.7 kPa) at a temperature in the region of 40° C.
5. customthe residue obtained
6. customis purified by HPLC (column
7. washeluent: elution gradient water-acetonitrile-TFA (0.07%) from 95-5 to 5-95 over 30 minutes)
8. additionThe fractions containing the desired product
9. concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the region of 40° C.