2-METHYL-3,4-DICHLOROPYRIDINE N-OXIDE

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of sodium methylate, prepared from 0.51 g of sodium and 20 ml of methanol, at -10° C. were added 3.5 g of 3,4-dichloro-2-picoline-N-oxide in 20 ml of anhydrous methanol. The mixture was allowed to warm slowly to room temperature and was then heated to reflux for 1 hour. The solvent was now removed by distillation under reduced pressure, water was added to the residue, the mixture was extracted with dichloromethane, and the solvent was evaporated off. Colorless crystals from diisopropyl ether, melting point 94°-97° C. was then heated to reflux for 1 hour The solvent was now removed by distillation under reduced pressure, water was added to the residue the mixture was extracted with dichloromethane the solvent was evaporated off

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of sodium methylate, prepared from 0.51 g of sodium and 20 ml of methanol, at -10° C. were added 3.5 g of 3,4-dichloro-2-picoline-N-oxide in 20 ml of anhydrous methanol. The mixture was allowed to warm slowly to room temperature and was then heated to reflux for 1 hour. The solvent was now removed by distillation under reduced pressure, water was added to the residue, the mixture was extracted with dichloromethane, and the solvent was evaporated off. Colorless crystals from diisopropyl ether, melting point 94°-97° C. was then heated to reflux for 1 hour The solvent was now removed by distillation under reduced pressure, water was added to the residue the mixture was extracted with dichloromethane the solvent was evaporated off

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of sodium methylate, prepared from 0.51 g of sodium and 20 ml of methanol, at -10° C. were added 3.5 g of 3,4-dichloro-2-picoline-N-oxide in 20 ml of anhydrous methanol. The mixture was allowed to warm slowly to room temperature and was then heated to reflux for 1 hour. The solvent was now removed by distillation under reduced pressure, water was added to the residue, the mixture was extracted with dichloromethane, and the solvent was evaporated off. Colorless crystals from diisopropyl ether, melting point 94°-97° C. was then heated to reflux for 1 hour The solvent was now removed by distillation under reduced pressure, water was added to the residue the mixture was extracted with dichloromethane the solvent was evaporated off