반응 #417945

반응 방정식

5-bromo-2-ethoxy-pyridine

urea hydrogen peroxide

→

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

용매

DCM

반응 조건

후처리

1. 1
   workup.ADDITIONare added
2. 2
   온도Afterwards cooling
3. 3
   기타is removed
4. 4
   기타The solvent is removed in vacuo, water
5. 5
   workup.ADDITIONis added
6. 6
   추출the resulting mixture is extracted with DCM
7. 7
   건조layers are dried over MgSO4
8. 8
   여과filtered
9. 9
   기타the sovent is removed in vacuo
10. 10
    기타The crude product is purified by column chromatography (silica gel, DCM/MeOH)

실험 절차

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).

출처