反应详情

温度

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