HRID1634202
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 solution of 1-tert-butoxycarbonyl-3-bromopiperidin-4-one (8 g) and thiobenzamide (3.4 g) in DMF was heated at 70 ° C. for 16 h, then cooled to room temperature. The solvent was evaporated in vacuo and the residue dissolved in water (100 ml) and washed with ether (100 ml), then basified with sodium hydroxide and extracted into ethyl acetate (3×100 ml). The solvent was dried (MgSO4) and evaporated to give the title compound as cream solid (2.81 g, 53% based on thiobenzamide used).
WORKUP
后处理
- customThe solvent was evaporated in vacuo
- dissolutionthe residue dissolved in water (100 ml)
- washwashed with ether (100 ml)
- extractionextracted into ethyl acetate (3×100 ml)
- dry with materialThe solvent was dried (MgSO4)
- customevaporated