Реакция #220198

ord-5f81c07103d8477b9ab602dbda118848

Уравнение реакции

O=CC(=O)c1ccccc1
Phenyl glyoxal
N#CCC(=O)NN
cyanoacetohydrazide
N#Cc1c(-c2ccccc2)cn[nH]c1=O
3-Oxo-5-phenyl-2,3-dihydro-pyridazine-4-carbonitrile

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooling
  2. 2
    Другоеthe solvent was evaporated
  3. 3
    Другоеthe crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane)
  4. 4
    ДругоеThe still impure product was further recrystallized from methanol affording 70 mg pure product

Методика

Phenyl glyoxal (1.0 g, 7.46 mmol) and cyanoacetohydrazide (740 mg, 7.46 mmol) were heated to reflux in 10 mL ethanol for 16 hours. After cooling, the solvent was evaporated and the crude brown mixture was purified by silica chromatography (1:9 methanol/dichloromethane). The still impure product was further recrystallized from methanol affording 70 mg pure product.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07390808B2uspto-grants-2008_06