反应详情

温度

160 °C

A mixture of 1.57 g (0.01 moles) 3-chloro-6-dimethylaminopyridazine and 2.08 g (0.02 moles) monocarbethoxyhydrazine is warmed up for half an hour at 160° C. The resulting mixture is cooled, water added thereto, the solid which separates filtered away and the filtrate neutralized with NaHCO3 until a final pH 7. The mixture is then extracted with chloroform; the organic extract dried over sodium sulphate and the solvent evaporated. The residual oil is purified by chromatography on silica gel, eluting with a mixture of chloroform:methanol 8.5:1.5. The unitary fractions on thin layer chromatography with the same Rf are collected together, evaporated and the residue treated while warm with ethyl ether, and the residue filtered off. By addition of hydrogen chloride to the filtrate, 3-(2-carbethoxyhydrazino)-6-dimethylaminopyridazine hydrochloride precipitates with good yields melting at 215°-217° C (with dec).

1. temperatureThe resulting mixture is cooled
2. filtrationthe solid which separates filtered away
3. extractionThe mixture is then extracted with chloroform
4. extractionthe organic extract
5. dry with materialdried over sodium sulphate
6. customthe solvent evaporated
7. customThe residual oil is purified by chromatography on silica gel
8. washeluting with a mixture of chloroform:methanol 8.5:1.5
9. customThe unitary fractions on thin layer chromatography with the same Rf are collected together
10. customevaporated
11. additionthe residue treated
12. temperaturewhile warm with ethyl ether
13. filtrationthe residue filtered off
14. additionBy addition of hydrogen chloride to the filtrate, 3-(2-carbethoxyhydrazino)-6-dimethylaminopyridazine hydrochloride
15. customprecipitates
16. customwith good yields melting at 215°-217° C (with dec)