HRID1829183
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
Sodium hydride (2.2 g, 80% dispersion in mineral oil, 73.2 mmol) was added to an ice-cooled solution of (3R)-N-tert-butoxycarbonylpyrrolidin-3-ol (J. Med. Chem. 41; 25; 1998; 4983) (12.5 g, 66.7 mmol) in tetrahydrofuran (330 ml), and the solution stirred at room temperature for an hour. Methyl iodide (14.5 g, 100 mmol) was then added and the reaction stiired for 18 hours. Water (100 ml) was added and the mixture concentrated under reduced pressure to remove the organic solvents. The aqueous was extracted with ethyl acetate, the combined organic solutions dried (MgSO4) and evaporated under reduced pressure to give the title compound as an oil, 12.48 g.
WORKUP
后处理
- concentrationthe mixture concentrated under reduced pressure
- customto remove the organic solvents
- extractionThe aqueous was extracted with ethyl acetate
- dry with materialthe combined organic solutions dried (MgSO4)
- customevaporated under reduced pressure