反应详情

To a solution of thieno[3,2-c]pyridine-2-carboxylic acid (D′-1) (11.5 g, 64.2 mmol) in DCM (200 mL) and DMF (50 mL) was added Et3N (19.5 g, 26.6 mL, 192.6 mmol) followed by HATU (36.6 g, 96.3 mmol). The reaction solution was stirred at room temperature for 20 mins, and then treated with N,O-dimethylhydroxylamine hydrochloride (6.9 g, 70.6 mmol). Stirring continued overnight at room temperature. The solvent was removed. The residue was dissolved in EtOAc and washed with water and brine. The organic layer was dried and concentrated. The residue was purified by chromatography on silica gel to give the title compound. MS (m/z): 223 (M+1)+.

1. stirringStirring
2. waitcontinued overnight at room temperature
3. customThe solvent was removed
4. dissolutionThe residue was dissolved in EtOAc
5. washwashed with water and brine
6. customThe organic layer was dried
7. concentrationconcentrated
8. customThe residue was purified by chromatography on silica gel