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
CDI (27.6 mmol, 4.47 g) was added portion wise to a stirring solution of o-nitrophenyl acetic acid (27.6 mmol, 5.00 g) in ethyl acetate (20 mL) at room temperature. The mixture was left stirring for 1 h and then was sequentially added of a solution of 4-Aminomethyl-cyclohexanecarboxylic acid methyl ester hydrogen chloride salt in ethyl acetate (20 mL), triethyl amine (72.5 mmol, 10 mL), DCM (5 mL) and acetone (5 mL). The final mixture was stirred at room temperature overnight. The reaction mixture was filtered through a paper filter, the filtered solution was washed with a (1N) NaOH (2×15 mL) and then with brine, the organic phase was dried over anhydrous Na2SO4, the solvent was removed under reduced pressure to obtain the titled compound. (8.2 g, 90%).
WORKUP
后处理
- waitThe mixture was left
- filtrationThe reaction mixture was filtered through a paper
- filtrationfilter
- washthe filtered solution was washed with a (1N) NaOH (2×15 mL)
- dry with materialwith brine, the organic phase was dried over anhydrous Na2SO4
- customthe solvent was removed under reduced pressure