تفاعل #938707

ord-046629c6c6284468b016c72af451f03e

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةis heated to the reflux temperature for two hours
  2. 2
    أخرىthe obtained precipitate is collected
  3. 3
    أخرىcrystallized from ethyl ether

الإجراء التجريبي

A mixture of water (300 ml), 3,6-dichloropyridazine (29.8 g; 0.2 mole), methylhydrazine (9.2 g; 0.2 mole), and sodium bicarbonate (17.8 g; 0.2 mole), is heated to the reflux temperature for two hours. After cooling to about 60° C., acetonylacetone (22.2 g; 0.2 mole) is added and stirring is prosecuted for further 1 hour. Then the mixture is neutralized with hydrochloric acid and the obtained precipitate is collected and crystallized from ethyl ether, yielding 28 g (59.2%) of 6-chloro-N-(2,5-dimethyl-1H-pyrrol-1-yl)-N-methyl-3-pyridazineamine, whose structure is confirmed by I.R. and NMR spectra. M.p. 93°-94.5° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04385179uspto-grants-1983_05