反应详情

A solution of 2-(3,5-difluoro-phenoxy)-nicotinic acid (0.300 grams, 1.19 mmole), 2-(4-Aminomethyl-phenyl)-propan-2-ol (0.197 grams, 1.19 mmole) and 1-hydroxybenzotriazole hydrate (0.177 grams, 1.31 mmole) in dry dimethylformamide was added 1-(3-dimethylamino)-propyl)-3-ethylcarbodiimide hydrochloride (0.273 grams, 1.43 mmole) and stirred over night. The mixture was poured into 100 ml water and extracted with ethyl acetate. The combined extracts were washed with 1 N NaOH, water and brine, dried over MgSO4, filtered and concentrated to give an oil that was purified by chromatography on silica eluting with 40% ethyl acetate/hexane to give an oil. Recrystalization from ethyl acetate/hexane gave a white solid (0.328 g). M.P. 68-70° C.; Anal. calcd. for C22H20N2O3F2: C, 66.32; H, 5.06; N, 7,03; N, 703. Found: C, 67.30; H, 5.39; N, 6.56.

1. extractionextracted with ethyl acetate
2. washThe combined extracts were washed with 1 N NaOH, water and brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customto give an oil that
7. customwas purified by chromatography on silica eluting with 40% ethyl acetate/hexane
8. customto give an oil
9. customRecrystalization from ethyl acetate/hexane