Реакция #417945

Уравнение реакции

5-bromo-2-ethoxy-pyridine

urea hydrogen peroxide

→

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

Растворители

DCM

Условия реакции

Обработка

1. 1
   workup.ADDITIONare added
2. 2
   ТемператураAfterwards cooling
3. 3
   Другоеis removed
4. 4
   ДругоеThe solvent is removed in vacuo, water
5. 5
   workup.ADDITIONis added
6. 6
   Экстракцияthe resulting mixture is extracted with DCM
7. 7
   Сушкаlayers are dried over MgSO4
8. 8
   Фильтрацияfiltered
9. 9
   Другоеthe sovent is removed in vacuo
10. 10
    ДругоеThe crude product is purified by column chromatography (silica gel, DCM/MeOH)

Методика

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).

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