HRID453844
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 containing 130 mg (0.45 mmol) of 1-(2,3-dihydro-benzo[1,4]dioxin-2-ylmethyl)-5-oxo-pyrrolidine-3-carboxylic acid methyl ester in dry tetrahydrofuran (4 mL) was added 68 mg (1.79 mmol) of LiAlH4. The reaction mixture was stirred at room temperature for 2½ h, and subsequently refluxed for 2 h. After the reaction mixture was cooled to room temperature, it was quenched with water and 1 M NaOH. The solution was filtered through celite and the filtrate was evaporated to dryness. Purification by column chromatography (silica gel, triethylamine/ethyl acetate, 1:99) afforded the title compound.
WORKUP
后处理
- temperaturesubsequently refluxed for 2 h
- temperatureAfter the reaction mixture was cooled to room temperature
- customit was quenched with water and 1 M NaOH
- filtrationThe solution was filtered through celite
- customthe filtrate was evaporated to dryness
- customPurification by column chromatography (silica gel, triethylamine/ethyl acetate, 1:99)