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% wt 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 6-chloro-5-methyl-nicotinic acid (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