反应详情

To a suspension of 25.4 g. (365 mmole) of hydroxylamine hydrochloride in one liter of methyl alcohol were added 39.4 g. (730 mmole) of sodium methylate. A slight exotherm occurred and sodium chloride precipitated. The solution was allowed to cool to room temperature, 50 ml. (365 mmole) of methyl 2-pyridinecarboxylate were added, and the reaction mixture was stirred overnight. The mixture was filtered to remove the salt precipitate and the filtrate was evaporated to dryness. The residue was dissolved in 100 ml. of water, pH 10.1, the solution acidified to pH 5.0 with concentrated hydrochloric acid. The solution was diluted with 500 ml. of isopropyl alcohol added dropwise and the additional sodium chloride precipitate was filtered. The filtrate was concentrated to about 100 ml. and the insoluble product was filtered. There were obtained 37.1 g. of the product which melted at about 58° C. to about 68° C. On chilling the filtrate an additional 12.5 g. of the product were obtained.

1. additionTo a suspension of 25.4 g
2. customsodium chloride precipitated
3. filtrationThe mixture was filtered
4. customto remove the salt precipitate
5. customthe filtrate was evaporated to dryness
6. dissolutionThe residue was dissolved in 100 ml
7. additionThe solution was diluted with 500 ml
8. additionof isopropyl alcohol added dropwise
9. filtrationthe additional sodium chloride precipitate was filtered
10. concentrationThe filtrate was concentrated to about 100 ml
11. filtrationand the insoluble product was filtered
12. customThere were obtained 37.1 g
13. temperatureOn chilling the filtrate an additional 12.5 g
14. customof the product were obtained