Triethylamine → 2-(4-Fluoro-phenoxy)-N-(5-oxo-morpholin-2-ylmethyl)-nicotinamide

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反応手順

A solution of 6-Aminomethyl-morpholin-3-one hydrochloride (0.200 grams, 1.2 mmole) and triethyl amine (0.150 grams, 1.5 mmole) in dimethylformamide was stirred at room temperature for 30 minutes. To the stirring solution 2-(4-Fluoro-phenoxy)-nicotinic acid (0.280 grams, 1.2 mmole), 1-hydroxybenzotriazole hydrate (0.237 grams, 1.755 mmole) and 2-diethylaminoethyl chloride hydrochloride (0.30 grams, 1.56 mmole) was added and stirred over night. The mixture was diluted with 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 a white solid which was purified by chromatography on silica eluting with 5% methanol/methylene chloride. Recrystalization from ethyl acetate/hexane gave white crystals. (0.175 g); M.P. 157-159° C.; Anal. calcd. for C17H16N3O4F: C, 59.14; H, 4.67; N, 12.17. Found: C, 59.00; H, 4.69; N, 12.19.

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