反应详情

Then, a solution of 2-aminonicotinic acid (3.0 g, 21.7 mmol) in N,N-dimethylformamide (30 mL) was cooled with an ice water, 1-hydroxybenzotriazole (3.51 g, 26 mmol), (3-dimethylaminopropyl)-ethyl-carbodiimide (4.04 g, 26 mmol) and a solution of the resulting 4-aminomethyl-phenol (3.0 g, 21.7 mmol) in N,N-dimethylformamide (20 mL) were added, and the solution was stirred for 18 hours at this temperature. The reaction solution was partitioned into brine, the organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was dissolved in ethyl acetate, filtration was carried out using NH silica gel, and the filtrate was concentrated. The residue was dissolved in methanol (90 mL), 1N sodium hydroxide (17.8 mL, 17.8 mmol) was added thereto, followed by stirring at room temperature for an hour and a half. The reaction solution was concentrated in vacuo, and the title compound (5.66 g) was obtained as a pale yellow solid.

1. customThe reaction solution was partitioned into brine
2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
3. customthe solvent was evaporated
4. dissolutionThe residue was dissolved in ethyl acetate
5. filtrationfiltration
6. concentrationthe filtrate was concentrated
7. dissolutionThe residue was dissolved in methanol (90 mL)
8. stirringby stirring at room temperature for an hour
9. concentrationThe reaction solution was concentrated in vacuo