反应详情

To ethyl 5-(3-aminophenyl)isoxazole-3-carboxylate (0.224 mmole) and triethylamine (0.896 mmole) in methylenechloride (3 mL) was added 1-acetyl-piperidine-4-carbonyl chloride HCl salt (0.314 mmole) via syringe at ambient temperature. After two hours, 1N HCl was added and the mixture was extracted with methylene chloride (3×40 mL). The combined organics were washed with aqueous Na2CO3, dried with anhydrous Na2SO4, filtered, concentrated under vacuo and purified by flash chromatography (10–15% ethyl acetate/Hexane) to provide (68 mg) of the titled compound.

1. extractionthe mixture was extracted with methylene chloride (3×40 mL)
2. washThe combined organics were washed with aqueous Na2CO3
3. dry with materialdried with anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under vacuo
6. custompurified by flash chromatography (10–15% ethyl acetate/Hexane)