HRID390424

反应详情

EQUATION

反应方程式

HRID 390424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a round bottom flask was added N-(4-(4,6-dichloropyrimidin-2-ylthio)phenyl)-3,3,3-trifluoropropanamide (350 mg, 0.9 mmol), 1,2,4-thiadiazole-5-amine (100 mg, 0.9 mmol), xanthphos (50 mg, 0.1 mmol), Pd2 dba3 (50 mg, 0.05 mmol), NaCO3 (150 mg, 1.5 mmol) and dioxane(10 cm). The mixture was flushed with nitrogen and then brought to reflux for 2 hours. The mixture was filtered, partitioned between ethylacetate and bicarbonate. The organic layer was dried with magnesium sulfate, and concentrated to an oil, which was purified by column chromatography to yield the product as a yellow solid (127 mg, 34%)

WORKUP

后处理

  1. customThe mixture was flushed with nitrogen
  2. temperatureto reflux for 2 hours
  3. filtrationThe mixture was filtered
  4. custompartitioned between ethylacetate and bicarbonate
  5. dry with materialThe organic layer was dried with magnesium sulfate
  6. concentrationconcentrated to an oil, which
  7. customwas purified by column chromatography