HRID1748635

反应详情

EQUATION

反应方程式

HRID 1748635 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

1,4-Dioxane (2 ml) was added to 4-[4-(5-bromo-3-methylpyridin-2-yl)cyclohex-3-en-1-yl]morpholin-3-one (150 mg) described in Reference Example 187, 5-methyl-1-[5-(trifluoromethyl)pyridin-2-yl]-1H-pyrazole-4-carboxamide (115 mg) described in Reference Example 120, palladium (II) acetate (3.8 mg), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (14.8 mg) and cesium carbonate (195 mg) and stirred at 110° C. for five hours. After the reaction, the reaction solution was cooled to room temperature, a saturated aqueous solution of ammonium chloride was added and the precipitated solid was filtered. The resulted solid was purified with a silica gel column chromatography (chloroform/methanol), suspended and washed with ethanol to give the titled compound (169 mg) as a white solid.

WORKUP

后处理

  1. customAfter the reaction
  2. temperaturethe reaction solution was cooled to room temperature
  3. filtrationthe precipitated solid was filtered
  4. customThe resulted solid was purified with a silica gel column chromatography (chloroform/methanol)
  5. washwashed with ethanol