HRID1435837
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
PROCEDURE
实验过程
A solution of (5-methyl-3-phenyl-4-isoxazolyl)methylamine (2.4 g, 12.7 mmol) and 5-chloro-pyrazine-2-carboxylic acid methyl ester (2.2 g, 12.7 mmol) in DMSO (15 mL) was heated with microwave irradiation to 160° C. for 30 min. After cooling to room temperature the reaction mixture was extracted (ethyl acetate/water). The organic phase was dried over sodium sulfate, concentrated and chromatographed (SiO2, heptane:ethyl acetate=100:0 to 20:80). The oily product obtained was triturated with diisopropylether and ethyl acetate to afford the title compound (3.5 g, 84% as an off-white solid. MS: m/e=325.4 [M+H]+.
WORKUP
后处理
- extractionwas extracted (ethyl acetate/water)
- dry with materialThe organic phase was dried over sodium sulfate
- concentrationconcentrated
- customchromatographed (SiO2, heptane:ethyl acetate=100:0 to 20:80)
- customThe oily product obtained
- customwas triturated with diisopropylether and ethyl acetate