反应详情

Inject acetic anhydride (0.250 ml, 2.65 mmol) dropwise to a solution of crude 7-(3,5-bis-trifluoromethyl-benzylamino)-5-ethyl-6,7-dihydro-5H-thieno[3,2-b]pyridine-4-carboxylic acid isopropyl ester (0.120 g, 0.243 mmol) and pyridine (0.250 ml, 3.10 mmol) in dichloromethane (1 ml) at room temperature. Stir the mixture at room temperature for 16 h. Evaporate the solvents and purify the resulting reside using silica gel column chromatography (gradient eluent, 0-35% ethyl acetate in hexane) to provide the title compound (0.0290 g, 22%). MS (ES+): 559 (M+Na); (ES−): 535 (M−H). cl Example 2

1. customat room temperature
2. customEvaporate the solvents
3. custompurify the resulting reside