Methyl iodide → 3-Methoxy-6-methyl-2-nitropyridine

Temperatur

50 °C

Commercially available 6-Methyl-2-nitro-pyridin-3-ol (Aldrich) (5.09 g, 33 mmol) in acetone (50 mL) was treated with K2CO3 (5.47 g, 39.6 mmol) and MeI (3.09 mL, 49.5 mmol). The orange suspension was heated to 50° C. for 90 hours. After evaporation of the solvent in vacuo the crude mixture was treated with 1N NaOH (50 mL) and extracted with EtOAc (2×50 mL) the combined organic phases was washed with brine (2×50 mL), dried over Na2SO4, filtered and concentrated in vacuo. 3-Methoxy-6-methyl-2-nitro-pyridine was obtained as a yellow solid.

1. customAfter evaporation of the solvent in vacuo the crude mixture
2. additionwas treated with 1N NaOH (50 mL)
3. extractionextracted with EtOAc (2×50 mL) the combined organic phases
4. washwas washed with brine (2×50 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo

ORD-Eintrag

ord-dab24a7b0a0444a89e1c98eaca5075d2

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08829190B2