反应详情

KN(TMS)2 (812 mg, 3.85 mmol) in toluene (3.85 ml) is added at 0° C. to a solution of 2-(4-Fluorophenyl)-5-(4-tert.butoxycarbonyl-1-piperazinyl)imidazo[4,5-b]pyridine (1.4 g, 3.5 mmol) in DMF (7 ml). After stirring at room temperature for 30 min., 4-iodo-2-methylthiopyrimidine (970 mg, 3.85 mmol) in toluene (3.85 ml) is added and the reaction stirred at room temperature for 1 h. Toluene is evaporated, the reaction mixture heated to 120° C. for 18 h, poured on water and extracted with ethyl acetate (containing 5% EtOH) three times. The combined organic phases are washed with brine, dried over Na2SO4, filtered and evaporated to dryness. Purification over SiO2 (acetone/hexanes 20/80) renders the title compound (950 mg, 52%) as colorless foam.

1. stirringthe reaction stirred at room temperature for 1 h
2. customToluene is evaporated
3. temperaturethe reaction mixture heated to 120° C. for 18 h
4. additionpoured on water
5. extractionextracted with ethyl acetate (containing 5% EtOH) three times
6. washThe combined organic phases are washed with brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customevaporated to dryness
10. customPurification over SiO2 (acetone/hexanes 20/80)