反应详情

To a mixture of {trans-4-[(6-nitrothieno[3,2-b]pyridin-7-yl)amino]cyclohexyl}methanol (0.26 g, 0.84 mmol) and N,N-diisopropylethylamine (0.30 mL, 1.7 mmol) in methylene chloride (3 mL) was added methanesulfonyl chloride (0.085 mL, 1.1 mmol). The resulting mixture was stirred at room temperature for 2 h. After diluting with water, the mixture was extracted with dichloromethane. The organic layers were concentrated and purified on silica gel (eluting with 0 to 70% EtOAc in hexanes) to give the desired product (0.2 g, 61%). LCMS calculated for C15H20N3O5S2 (M+H)+: m/z=386.1. Found: 386.0.

1. extractionthe mixture was extracted with dichloromethane
2. concentrationThe organic layers were concentrated
3. custompurified on silica gel (eluting with 0 to 70% EtOAc in hexanes)