Phosphorus oxychloride → 2,6-Dichloro-4-methylpyridine

A mixture of 2-chloro-4-methyl-pyridine 1-oxide (1.0 g, 7.0 mmol) and phosphorus oxychloride (10 mL) was heated at reflux for 4 h. The volatiles were evaporated and the residue dissolved in ethyl acetate. The solution was washed with ice-water followed by sodium bicarbonate solution. The organic phase was again washed with water, brine solution, dried over anhydrous sodium sulfate and concentrated to obtain a residue which was purified by column chromatography over silica gel (60-120 mesh) using petroleum ether as eluent to afford 2,6-dichloro-4-methyl-pyridine (491 mg, 43%) as a white solid.

1. temperaturewas heated
2. temperatureat reflux for 4 h
3. customThe volatiles were evaporated
4. dissolutionthe residue dissolved in ethyl acetate
5. washThe solution was washed with ice-water
6. washThe organic phase was again washed with water, brine solution
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated
9. customto obtain a residue which
10. customwas purified by column chromatography over silica gel (60-120 mesh)

ORDレコード

ord-51cb4aae7be0496d84ff01fb90662113

出典データセット

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08524705B2