HRID1748636

反应详情

EQUATION

反应方程式

HRID 1748636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoroacetic acid (0.96 ml) was added at room temperature to a solution of 8-[5-({[5-methyl-1-(4-methylphenyl)-1H-pyrazol-4-yl]carbonyl}amino)pyridin-2-yl]-1,4-dioxaspiro[4.5]decane-8-carboxylic acid ethyl ester (1.27 g) described in Example D4 in dichloromethane (2.5 ml) and stirred at the same temperature for six hours. Trifluoroacetic acid (1.9 ml) was added at the same temperature and stirred at the same temperature for 18 hours. After the reaction, the solvent and trifluoroacetic acid were evaporated, a saturated aqueous solution of sodium bicarbonate was added and extracted with ethyl acetate twice. The organic solution was dried over anhydrous magnesium sulfate and concentrated to give 1-[5-({[5-methyl 1-(4-methylphenyl)-1H-pyrazol-4-yl]carbonyl}amino)pyridin-2-yl]-4-oxocyclohexanecarboxylic acid ethyl ester (1.09 g) as a white solid.

WORKUP

后处理

  1. stirringstirred at the same temperature for 18 hours
  2. customAfter the reaction
  3. customthe solvent and trifluoroacetic acid were evaporated
  4. additiona saturated aqueous solution of sodium bicarbonate was added
  5. extractionextracted with ethyl acetate twice
  6. dry with materialThe organic solution was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated