HRID538067

反应详情

EQUATION

反应方程式

HRID 538067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. waitThe mixture was left
  2. filtrationThe reaction mixture was filtered through a paper
  3. filtrationfilter
  4. washthe filtered solution was washed with a (1N) NaOH (2×15 mL)
  5. dry with materialwith brine, the organic phase was dried over anhydrous Na2SO4
  6. customthe solvent was removed under reduced pressure