HRID447101

反应详情

EQUATION

反应方程式

HRID 447101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of 1-(6-benzyl-4,5-dimethyl-pyridazin-3-yl)-4-methyl-piperidine-4-carboxylic acid ethyl ester (0.60 g, 1.6 mmol) in EtOH (5 mL) is added sodium hydroxide (0.5 g, 13.2 mmol) in H2O (5 mL). After being stirred at 25° C. for two hr, the mixture is concentrated, and extracted with CH2Cl2 (2×10 mL) to remove impurities. The aqueous layer is acidified by 1N HCl to pH ˜5, and extracted with CH2Cl2 (6×20 mL). The combined organic solution is dried over Na2SO4, filtered and concentrated to give 1-(6-benzyl-4,5-dimethyl-pyridazin-3-yl)-4-methyl-piperidine-4-carboxylic acid (0.49 g, 89%).

WORKUP

后处理

  1. concentrationthe mixture is concentrated
  2. extractionextracted with CH2Cl2 (2×10 mL)
  3. customto remove impurities
  4. extractionextracted with CH2Cl2 (6×20 mL)
  5. dry with materialThe combined organic solution is dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated