HRID1920908
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
- 0 °C
PROCEDURE
实验过程
To a solution of (5-methyl-3-pyridin-2-yl-isoxazol-4-yl)-methanol (465 mg, 2.44 mmol) in THF (10 mL) was added 3-oxo-2,3-dihydro-isoxazole-5-carboxylic acid methyl ester (350 mg, 2.45 mmol) and triphenylphosphine (769 mg, 2.93 mmol) at 0° C. under an argon atmosphere. Then diethyl azodicarboxylate (˜40% in toluene, 1.23 mL, 2.68 mmol) was added and the reaction mixture was stirred for 1 h at 0° C. and then overnight at room temperature. Concentration and purification by chromatography (silica, heptane:ethyl acetate=4:1 to 1:4) afforded the title compound (443 mg, 57%) as a white solid. MS: m/e=316.2 [M+H]+.
WORKUP
后处理
- customovernight
- customat room temperature
- concentrationConcentration and purification by chromatography (silica, heptane:ethyl acetate=4:1 to 1:4)