反应详情

To a solution of 2,6-diaminonicotinic acid described in Preparation Example A-15 (109 mg, 0.71 mmol) in dimethylsulfoxide (10 mL) were added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (272 mg, 1.42 mmol), 1-hydroxybenzotriazole (217 mg, 1.42 mmol) and C-(5-benzyloxy-thiophen-2-yl)methylamine described in Example E-76 (156 mg, 0.71 mmol), and the solution was stirred at room temperature for 14 hours. The reaction solution was poured into brine, extracted with ethyl acetate, the fractionated organic layer was dried over anhydrous magnesium sulfate and then concentrated. The obtained residue was subjected to NH silica gel column chromatography, eluted with solvent (ethyl acetate) and the title compound (157 mg, 0.44 mmol, 62%) was obtained.

1. extractionextracted with ethyl acetate
2. dry with materialthe fractionated organic layer was dried over anhydrous magnesium sulfate
3. concentrationconcentrated
4. washeluted with solvent (ethyl acetate)