反应详情

温度

50 °C

Stir at 50° C. a mixture of 3-(4-pyridinylamino)-1H-indole-2-carboxylic acid potassium salt (1.0 g, 3.43 mmol), KI (0.16 g) 2,2-dimethyl-propionic acid chloromethyl ester (0.63 g, 4.16 mmol) in DMF (20 mL) for 1.5 h. Cool, and partition between H2O-EtOAc. Wash the extract with aqueous NaHCO3 solution, dry the extract (MgSO4), filter and concentrate under vacuum to afford the crude product. Chromatography the product on a silica gel column eluting with 8% MeOH/EtOAc to obtain 0.64 g of the title compound as a solid; MS 326(M+H), m.p. 223–224° C. TLC (silica gel, 8% MeOH/EtOAc) Rf=0.30.

1. temperatureCool
2. custompartition between H2O-EtOAc
3. washWash the
4. extractionextract with aqueous NaHCO3 solution
5. customdry the
6. extractionextract (MgSO4)
7. filtrationfilter
8. concentrationconcentrate under vacuum
9. customto afford the crude product
10. washChromatography the product on a silica gel column eluting with 8% MeOH/EtOAc