反应详情

In a round bottomed flask, dissolve methanesulfonic acid 2-[3-tert-butyl-5-(3-{4-[7-(4-methanesulfonyl-phenyl)-imidazo[1,2-a]pyridin-3-yl]-benzyl}-ureido)-pyrazol-1-yl]-ethyl ester (75 mg, 0.11 mmol) in DMF (2 mL). Add morpholine (0.1 mL, 10 eq) and heat the reaction to 70° C. overnight under N2. Dilute the reaction with EtOAc then wash with water, 1 N NaOH, and saturated aqueous saturated sodium chloride. Dry the organics over magnesium sulfate, filter, and concentrate. Purify the compound on a silica gel column (EtOAc to 5% MeOH: DCM to 10% 2 M NH3 in MeOH: DCM) to give a pale yellow solid (46 mg, 62%). MS (ES), m/z 656 (M+1).

1. customthe reaction to 70° C. overnight under N2
2. additionDilute
3. washthen wash with water, 1 N NaOH, and saturated aqueous saturated sodium chloride
4. dry with materialDry the organics over magnesium sulfate
5. filtrationfilter
6. concentrationconcentrate
7. customPurify the compound on a silica gel column (EtOAc to 5% MeOH: DCM to 10% 2 M NH3 in MeOH: DCM)