HRID2106760

反应详情

EQUATION

反应方程式

HRID 2106760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 13 parts of 1-[1-(4-morpholinyl)ethylidene-2-(4-nitrophenyl)hydrazine, 8.5 parts of 1-isocyanatopropane, 1 part of N,N-dimethyl-4-pyridinamine and 39 parts of dichloromethane was stirred and refluxed for 2 hours. The whole was evaporated and 90 parts of dimethylbenzene were added to the residue. Stirring at reflux was continued for 3 hours. The reaction mixture was cooled and filtered over diatomaceous earth. The filtrate was saturated with petroleum ether. The precipitated product was filtered off and crystallized from 2-propanol, yielding 8.5 parts (65%) of 2,4-dihydro-5-methyl-2-(4-nitrophenyl)-4-propyl-3H-1,2,4-triazol-3-one; mp. 125.4° C. (int. 20).

WORKUP

后处理

  1. temperaturerefluxed for 2 hours
  2. customThe whole was evaporated
  3. addition90 parts of dimethylbenzene were added to the residue
  4. stirringStirring
  5. temperatureat reflux
  6. temperatureThe reaction mixture was cooled
  7. filtrationfiltered over diatomaceous earth
  8. filtrationThe precipitated product was filtered off
  9. customcrystallized from 2-propanol