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 5-(2,4-dimethoxybenzyl)-4-oxo-5-azaspiro[2.4]heptane-7-carboxylic acid methyl ester (2.02 g) in tetrahydrofuran/methanol (1/1, 12 ml) was added a 1M aqueous solution of sodium hydroxide (12 ml) at room temperature, and the mixture was stirred for 1 hour. To this reaction solution was added a 2M aqueous solution of hydrochloric acid (6 ml), and the mixture was stirred, and then concentrated under reduced pressure. The resulting residue was dissolved in ethyl acetate, the solution was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. To the resulting solid was added diisopropyl ether (8 ml), and the mixture was stirred. A solid was collected from this suspension by filtration, and was dried under reduced pressure to give the titled compound (1.59 g).
WORKUP
后处理
- stirringthe mixture was stirred
- concentrationconcentrated under reduced pressure
- dissolutionThe resulting residue was dissolved in ethyl acetate
- washthe solution was washed with a saturated aqueous solution of sodium chloride
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- additionTo the resulting solid was added diisopropyl ether (8 ml)
- stirringthe mixture was stirred
- filtrationA solid was collected from this suspension by filtration
- customwas dried under reduced pressure