HRID249693

反应详情

EQUATION

反应方程式

HRID 249693 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(4-chloro-6-morpholin-4-yl-pyrimidin-2-yl)-2-methyl-butan-2-ol (3.3 g, 11.5 mmol) was dissolved in dioxane (30 mL). To the reaction mixture was added anhydrous hydrazine (7.5 mL, 220 mmol). The reaction was then heated at reflux for five hours. The solvent was removed under reduced pressure, and the crude solid was dissolved in a mixture of dichloromethane (800 mL) and 10% potassium carbonate (40 mL). The organic layer was isolated, dried with sodium sulfate, and evaporated to give 4-(4-hydrazino-6-morpholin-4-yl-pyrimidin-2-yl)-2-methyl-butan-2-ol (2.61 g, 9.2 mmol).

WORKUP

后处理

  1. temperatureThe reaction was then heated
  2. temperatureat reflux for five hours
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe crude solid was dissolved in a mixture of dichloromethane (800 mL) and 10% potassium carbonate (40 mL)
  5. customThe organic layer was isolated
  6. dry with materialdried with sodium sulfate
  7. customevaporated