反应详情

1.48 g (4.6 mmol) of 4-(3-chloro-anilino)-6-(pyrid-2-yl)-7H-pyrrolo[2,3-d]pyrimidine (see Example 1) are suspended in 115 ml of dioxane; with cooling, 46 ml of 0.1 N HCl solution (0.1 normal hydrochloric acid solution) are added and the reaction suspension is stirred at RT for 2.5 hours. The suspension is concentrated by evaporation and the residue is stirred in 400 ml of hot methanol and filtered. The filtrate is filtered while hot through activated carbon, concentrated by evaporation and digested in cold ethanol; m.p. 276-278° C.; 1H-NMR (200 MHz, DMSO-d6): 13.1 and 10.7 (2s, 2H), 8.71 (d, J=5, 1H), 8.45 and 8.08 (2s, 2H), 8.00 (m, 2H), 7.76 (d, J=8, 1H), 7.68 (s, 1H), 7.50 (d, J=8, 1H), 7.42 (m, 1H), 7.27 (d, J=8, 1H).

1. temperaturewith cooling
2. concentrationThe suspension is concentrated by evaporation
3. stirringthe residue is stirred in 400 ml of hot methanol
4. filtrationfiltered
5. filtrationThe filtrate is filtered while hot
6. concentrationconcentrated by evaporation