HRID2384509
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction was then heated
- temperatureat reflux for five hours
- customThe solvent was removed under reduced pressure
- dissolutionthe crude solid was dissolved in a mixture of dichloromethane (800 mL) and 10% potassium carbonate (40 mL)
- customThe organic layer was isolated
- dry with materialdried with sodium sulfate
- customevaporated