反应详情

A quantity of 0.065 g (0.14 mmol) of {4-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino]phenyl}-acetic acid, methyl ester of Example 84 was dissolved in 25 mL of hot methanol with stirring. At the boiling point, 1 mL of 2N sodium hydroxide was added. After 1 hour reflux, the solution was concentrated to 5 mL volume (solid was out of solution). Water (10 mL) was added to give a complete solution. Glacial acetic acid (0.25 mL) was added to precipitate the solid free acid product. The solid was filtered, washed well with water, and dried; wt 0.060 g. Purification was accomplished by dissolution in 60 mL of 50% methanol/methylene chloride. Traces of solids were filtered, and the filtrate was concentrated with stirring to 2 mL volume. The separated solid was filtered and washed with 0.5 mL of methanol and ether; wt 0.050 g; mp 286°-290° C.

1. temperatureAfter 1 hour reflux
2. concentrationthe solution was concentrated to 5 mL volume (solid was out of solution)
3. additionWater (10 mL) was added
4. customto give a complete solution
5. customto precipitate the solid free acid product
6. filtrationThe solid was filtered
7. washwashed well with water
8. customdried
9. customPurification
10. dissolutionwas accomplished by dissolution in 60 mL of 50% methanol/methylene chloride
11. filtrationTraces of solids were filtered
12. concentrationthe filtrate was concentrated
13. stirringwith stirring to 2 mL volume
14. filtrationThe separated solid was filtered
15. washwashed with 0.5 mL of methanol and ether