반응 #328989

ord-f7289e6e9b8046b188b486e0dee49891

반응 방정식

COC(=O)CC(=O)C(=NNc1ccc(OC)c(OC)c1)C(=O)OC
hydrazone
COC(=O)CC(=O)C(=NNc1ccc(OC)c(OC)c1)C(=O)OC
2-[(3,4-Dimethoxy-phenyl)-hydrazono]-3-oxo-pentanedioic acid dimethyl ester
C1CCCCC1
cyclohexane
COC(=O)c1nn(-c2ccc(OC)c(OC)c2)c(=O)cc1O
dihydropyridazine ester
수율 65.2%
COC(=O)c1nn(-c2ccc(OC)c(OC)c2)c(=O)cc1O
1-(3,4-Dimethoxy-phenyl)-4-hydroxy-6-oxo-1,6-dihydro-pyridazine-3-carboxylic acid methyl ester
수율 65.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도to reflux in a sealed tube for 4 hours
  3. 3
    온도to cool
  4. 4
    기타to crystallize the desired product
  5. 5
    여과Filtration
  6. 6
    기타drying in vacuo

실험 절차

The hydrazone (28) (500 mg) was dissolved in dichlorobenzene and heated to reflux in a sealed tube for 4 hours. The reaction was allowed to cool and cyclohexane was added dropwise to crystallize the desired product. Filtration and drying in vacuo yielded the desired dihydropyridazine ester (29) (295 mg) as a solid. MS+: m/e=307.0 (M+H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08653088B2uspto-grants-2014_02