HRID1076665

反应详情

EQUATION

反应方程式

HRID 1076665 的结构方程式

PROCEDURE

实验过程

0.8 g. 3-(5-nitro-2-thienyl)-6-amino-s-triazolo[4,3-b]pyridazine was suspended in a mixture of 3 ml. N,N-dimethylformamide and 1. ml. N,N-dimethyl formamide-diethyl acetal and heated, while stirring, on a waterbath for two hours. Thereafter, the reaction mixture was cooled, solid material was filtered off with suction and the residue is washed with N,N-dimethyl formamide. There was thus obtained 0.4 g. (41% of theory) 3-(5-nitro-2-thienyl)-6-(diethylaminomethylene)-amino-s-triazolo[4,3-b]pyridazine (m.p. 247°-249°C). After recrystallization from N,N-dimethyl-formamide, with the addition of charcoal the product was obtained in the form of yellow crystals which melt at 249°-252°C. The elementary analyses and spectra confirm the structure.

WORKUP

后处理

  1. temperatureThereafter, the reaction mixture was cooled
  2. filtrationsolid material was filtered off with suction
  3. washthe residue is washed with N,N-dimethyl formamide
  4. customAfter recrystallization from N,N-dimethyl-formamide
  5. additionwith the addition of charcoal the product
  6. customwas obtained in the form of yellow crystals which
  7. custommelt at 249°-252°C