反应详情

温度

0 °C

A solution of 6-chloro-3-formyl-5-methyl-pyridine (10 g, 64 mmol) in formic acid (200 mL) is cooled at 0° C. and an aq. 50% weight solution of H2O2 in water (9.6 mL, 360 mmol) is added at this temperature. The mixture is stirred at 0° C. for 15 h, carefully diluted with water (200 mL) and extracted with DCM (8×100 mL). The combined org. extracts are washed with 1M aq. HCl (100 mL) (check for remaining peroxide), dried (MgSO4), filtered and evaporated. The residue is dried to give the title compound (9.56 g); LC-MS: tR=0.72 min, [M+1]+=172.0.

1. extractionextracted with DCM (8×100 mL)
2. washextracts are washed with 1M aq. HCl (100 mL) (check for remaining peroxide)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue is dried