反应 #554644

反应方程式

cyclobutanol

5-bromo-2-chloro-pyrimidine

NaH

→

5-Bromo-2-cyclobutoxy-pyrimidine

溶剂

dioxane

反应条件

后处理

1. 1
   其他After removing of the cooling bath the reaction mixture
2. 2
   其他The reaction is quenched by the addition of water and sat. aq. NaHCO3 solution
3. 3
   其他The dioxane is removed in vacuo
4. 4
   萃取the aq. residue is extracted with DCM
5. 5
   洗涤washed with water
6. 6
   干燥dried with MgSO4
7. 7
   过滤filtered
8. 8
   其他The solvent is removed under reduced pressure
9. 9
   其他The crude product is used without further purification

实验过程

2.42 mL (31.0 mmol) cyclobutanol and 3.00 g (15.5 mmol) 5-bromo-2-chloro-pyrimidine are added to 40 mL dioxane and cooled down to 0° C. Then the reaction mixture is charged with 1.86 g (46.5 mmol) NaH. After removing of the cooling bath the reaction mixture is stirred at r.t. for 1 h. The reaction is quenched by the addition of water and sat. aq. NaHCO3 solution. The dioxane is removed in vacuo and the aq. residue is extracted with DCM. The org. phases are combined, washed with water, dried with MgSO4 and filtered. The solvent is removed under reduced pressure. The crude product is used without further purification.

来源