反应 #417945

反应方程式

5-bromo-2-ethoxy-pyridine

urea hydrogen peroxide

→

3-Bromo-6-ethoxy-2-methoxy-pyridine

溶剂

DCM

反应条件

后处理

1. 1
   workup.ADDITIONare added
2. 2
   温度Afterwards cooling
3. 3
   其他is removed
4. 4
   其他The solvent is removed in vacuo, water
5. 5
   workup.ADDITIONis added
6. 6
   萃取the resulting mixture is extracted with DCM
7. 7
   干燥layers are dried over MgSO4
8. 8
   过滤filtered
9. 9
   其他the sovent is removed in vacuo
10. 10
    其他The crude product is purified by column chromatography (silica gel, DCM/MeOH)

实验过程

To 5.00 g (24.7 mmol) 5-bromo-2-ethoxy-pyridine in 50 mL DCM are added 4.66 g (49.5 mmol) urea hydrogen peroxide. Then the mixture is chilled to 0° C. before 6.88 mL (49.5 mmol) TFA anhydride are added. Afterwards cooling is removed and the resulting mixture is stirred over night while the temperature raises to r.t. The solvent is removed in vacuo, water is added and the resulting mixture is extracted with DCM. The combined org. layers are dried over MgSO4, filtered and the sovent is removed in vacuo. The crude product is purified by column chromatography (silica gel, DCM/MeOH).

来源