反应详情

A solution of tert-butyl {1-[({2-[(2,3-difluorobenzyl)thio]-6-methoxypyrimidin-4-yl}amino)sulfonyl]azetidin-3-yl}carbamate (the product of step ii, 0.48 g) and TFA (2 ml) in methanol (6 ml) was stirred at room temperature for 1.5 h then the volatiles evaporated and 7M ammonia in methanol (6 ml) added to the residue. The solution was stirred for 2 h then the volatiles evaporated and the residue purified by column chromatography on silica using a 2-8% mixture of methanol in DCM and then further purified by reverse phase HPLC (gradient 5-95% acetonitrile in 0.1% aqueous ammonium acetate) to afford the title compound as a white solid. Yield: 73 mg

1. customthe volatiles evaporated
2. addition7M ammonia in methanol (6 ml) added to the residue
3. customthe volatiles evaporated
4. customthe residue purified by column chromatography on silica using a 2-8% mixture of methanol in DCM
5. customfurther purified by reverse phase HPLC (gradient 5-95% acetonitrile in 0.1% aqueous ammonium acetate)