反应详情

To a solution of 3-(1-(3-fluorobenzyl)-1H-pyrazol-4-yl)-5-(4-(piperazin-1-yl)phenyl)-1-tosyl-1H-pyrrolo[2,3-b]pyridine hydrochloride (step 1 example 103) (150 mg. 0.233 mmol) in chloroform (10 mL) triethyl amine (0.16 mL, 1.165 mmol) was added at 0° C. drop wise. This solution was added to a solution of triphosgene (59 mg, 0.233 mmol) in chloroform (10 mL) and stirred at RT for 30 minutes. Ammonia in THF was added to this solution drop wise and stirred at RT overnight. This was diluted with water and extracted in chloroform and distilled out the solvent to afford the 40 mg (26.4% yield) of the titled compound after purification with preparative TLC (silicagel-1000 micron) using 3% methanol in DCM as eluent. MS: m/z=649.7 (M+1).

1. stirringstirred at RT overnight
2. extractionextracted in chloroform
3. distillationdistilled out the solvent