HRID923492
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
To a solution of 430 mg of 3-(tert-butoxycarbonyl)-2,2,4-trimethyl-1,3-oxazolidine-4-carboxylic acid in 4 ml of DMF was added 296 mg of 1,1′-carbonyldiimidazole, followed by stirring at room temperature for 2 hours. To the reaction mixture was added 146 mg of N-hydroxyacetamidine, followed by stirring at room temperature for 1 hour, at 110° C. for 2 hours, and then at 130° C. overnight. The reaction mixture was left to be cooled to room temperature and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 390 mg of tert-butyl 2,2,4-trimethyl-4-(3-methyl-1,2,4-oxadiazol-5-yl)-1,3-oxazolidine-3-carboxylate.
WORKUP
后处理
- stirringby stirring at room temperature for 1 hour, at 110° C. for 2 hours
- customat 130° C.
- customovernight
- waitThe reaction mixture was left
- temperatureto be cooled to room temperature
- customthe solvent was evaporated under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography