Hydrogen Peroxide → 2-Chloro-4-methylpyridine 1-oxide

Temperatur

65 °C

2-chloro-4-methylpyridine (10 g, 80 mmol) was dissolved in acetic acid (100 ml). Hydrogen peroxide (31%, 86.8 g, 80.7 ml, 790 mmol)) was added in 4 portions and the solution stirred under nitrogen at 65° C. for 18 hours. The mixture was poured into ice water (300 ml), and solid Na2CO3 added until the solution was alkaline. The mixture was extracted with DCM (3×300 ml), the organic fractions combined, washed with sodium thiosulfate (1M, 100 ml), brine, dried over Na2SO4, and the volatiles removed in vacuum to give the titled compound.

1. additionadded until the solution
2. extractionThe mixture was extracted with DCM (3×300 ml)
3. washwashed with sodium thiosulfate (1M, 100 ml), brine
4. dry with materialdried over Na2SO4
5. customthe volatiles removed in vacuum

ORD-Eintrag

ord-6a615a75ed284508a0b89c6529a24c42

Quelldatensatz

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08552022B2