HRID38544

反应详情

EQUATION

反应方程式

HRID 38544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

tert-Butyl 4-{[3-chloro-4-(pyridin-2-ylmethoxy)phenyl]amino}-3-cyano-5,8-dihydrothieno[2,3-b:5,4-c′]dipyridine-7(6H)-carboxylate from Example 56A (210 mg, 0.34 mmol) was dissolved in 2-propanol, and 4 M gaseous hydrogen chloride in dioxane (0.17 mL, 0.67 mmol) was added. The mixture was heated to 80° C. for 3 h. The precipitate was collected by suction filtration and dissolved in diluted aqueous sodium hydroxide solution. Some methanol was added, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and the solvent was evaporated. The title compound was crystallized from dichloromethane/diethyl ether to yield 116 mg (77%).

WORKUP

后处理

  1. filtrationThe precipitate was collected by suction filtration
  2. dissolutiondissolved in diluted aqueous sodium hydroxide solution
  3. additionSome methanol was added
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customthe solvent was evaporated
  7. customThe title compound was crystallized from dichloromethane/diethyl ether
  8. customto yield 116 mg (77%)