反应详情

To a stirred solution of 2 equivalents of 3-Amino-2,2-dimethyl-propan-1-ol (1.0 g, 10 mmol) in DMF in the presence of 2 equivalents of DIEA (1.7 ml, 10 mMol) is added a solution of sulfonylchloride (1b) (1.75 g, 5 mMol, 1 equivalent) in DMF. The reaction mixture is stirred for 12 h at room temperature. DCM is added and any excess of amine is extracted into 0.1N HCl solution. The organic phase is washed with brine and dried over MgSO4. 4-Chloro-N-[5-(3-hydroxy-2,2-dimethyl-propylsulfamoyl)-thiophen-2-ylmethyl]-benzamide (compound of formula XII) is obtained after evaporation of the solvent. LC-MS analysis and NMR analysis showed that the compound was pure enough to carry on the next step.

1. extractionany excess of amine is extracted into 0.1N HCl solution
2. washThe organic phase is washed with brine
3. dry with materialdried over MgSO4