反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
To a solution of ethyl 5-cyclopropyl-3-(3,5-dichloro-4-pyridinyl)-4-isoxazolecarboxylate (210 mg, 0.642 mmol) in 2:1 tetrahydrofuran:methanol (3 mL) was added 1 N sodium hydroxide (0.963 mL, 0.963 mmol). The solution was heated in a microwave reactor to 120° C. for 500 seconds. Then 1 N hydrochloric acid (0.963 mL, 0.963 mmol) was added and the solution was concentrated. The residue was taken up with water and extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate and concentrated to afford 5-cyclopropyl-3-(3,5-dichloro-4-pyridinyl)-4-isoxazolecarboxylic acid (158 mg, 82%). 1H-NMR (400 MHz, DMSO-d6) δ 13.35 (s, 1H), 8.81 (s, 2H), 2.91-2.84 (m, 1H), 1.34-1.24 (m, 4H).
WORKUP
后处理
- concentrationthe solution was concentrated
- extractionextracted twice with ethyl acetate
- washThe combined organic layers were washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated