反应详情

A mixture of ethyl 5-methoxy-2-methylindolin-3-ylacetate (2.0g.), 6-chloro-4-methyl-2-phenylpyrimidine (1.76g.) and concentrated hydrochloric acid (0.5ml.) in ethanol (50ml.) was heated under reflux for 5 hours. The solution was cooled, saturated sodium acetate solution (3ml.) was added, and the mixture was concentrated in vacuo. The residue was diluted with water (30ml.) and extracted with ethyl acetate (3 × 30ml.). The combined exracts were washed with water and then dried (Na2SO4), and the solvent was evaporated in vacuo at ca 50° C. to give ethyl 5-methoxy-2-methyl-1-(4-methyl-2-phenylpyrimidin-6-yl)indolin-3-ylacetate as a syrup. This was shown to be pure by TLC (System A) and by NMR spectroscopy (OCH3 at 6.23τ).

1. temperaturewas heated
2. temperatureunder reflux for 5 hours
3. temperatureThe solution was cooled
4. concentrationthe mixture was concentrated in vacuo
5. additionThe residue was diluted with water (30ml.)
6. extractionextracted with ethyl acetate (3 × 30ml.)
7. washThe combined exracts were washed with water
8. dry with materialdried (Na2SO4)
9. customthe solvent was evaporated in vacuo at ca 50° C.