反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 2-(adamantan-2-yl)-4,4-dimethyl-1,2-diazetidin-3-one (50.0 mg, 0.213 mmol) prepared in Process 3 of Example 12 in dichloromethane was added with 3-fluoro-2-methylbenzoic acid (32.8 mg, 0.213 mmol), diisopropylethylamine (82.6 mg, 0.639 mmol) and PyBOP (133 mg, 0.256 mmol) at room temperature, and the resultant was stirred at the same temperature for 18 hours. The reaction solution was added with water and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo, the obtained residue was purified using Preparative Thin-Layer chromatography (hexane:ethyl acetate=2:1), and the title compound (6.90 mg, 8.70%) was obtained as a white crystalline solid.
WORKUP
后处理
- extractionextracted with chloroform
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customthe obtained residue was purified