반응 #56174

ord-8f3ad70dcc0149729543ac45493e93d6

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도is heated
  2. 2
    온도to reflux for 9 hours
  3. 3
    온도after cooling the mixture
  4. 4
    추출The solution is extracted with 3×50 ml of chloroform
  5. 5
    건조the combined organic phases are dried over magnesium sulphate
  6. 6
    기타After evaporation the residue
  7. 7
    기타is recrystallized from a 3:1 mixture of isopropanol and petroleum ether

실험 절차

A mixture of 4.17 g (0.02 moles) of 3-chloro-6-(3,5-dimethyl-1-pyrazolyl)-pyridazine, 42 ml of ethanol and 2.3 g (0.05 moles) of methyl hydrazine is heated to reflux for 9 hours, and after cooling the mixture is poured into 100 ml of water. The solution is extracted with 3×50 ml of chloroform and the combined organic phases are dried over magnesium sulphate. After evaporation the residue is recrystallized from a 3:1 mixture of isopropanol and petroleum ether. Yield: 1.9 g (44.5%); m.p.: 93°-94° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04224325uspto-grants-1980_09