HRID731643
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 mixture of [2-(5-methyl-3-phenyl-isoxazol-4-yl)-imidazo[1,2-a]pyridin-7-yl]-carbamic acid tert-butyl ester (1.0 g, 2.56 mmol) in hydrochloric acid (4 M in dioxane, 29 mL) was stirred at room temperature for 6 h. The precipitate was then filtered off and dissolved in a dilute solution of sodium hydrogen carbonate and then extracted with ethyl acetate. The organic layer was then washed with brine and then dried over sodium sulphate and evaporated to leave a brown foam. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 25:75) afforded the title compound (477 mg, 64%) which was obtained as a light brown foam. MS: m/e=291.1 [M+H]+.
WORKUP
后处理
- filtrationThe precipitate was then filtered off
- dissolutiondissolved in a dilute solution of sodium hydrogen carbonate
- extractionextracted with ethyl acetate
- washThe organic layer was then washed with brine
- dry with materialdried over sodium sulphate
- customevaporated
- customto leave a brown foam
- customPurification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 25:75)