HRID963153

反应详情

EQUATION

反应方程式

HRID 963153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloro-3-nitropyridine (100 g, 0.63 mol), hydrazine monohydrate (70.4 mL, 72.6 g, 1.45 mol) and methanol (1.3 L) were mixed and heated to reflux with stirring. After 30 min the reaction mixture was cooled and filtered collecting the insoluble materials. The filtrate was concentrated by evaporation under reduced pressure and the residue obtained as well as the insoluble materials from the filtration were diluted with water. The insoluble solids present were collected by filtration, washed with water, and dried to obtain 95.2 g (98 percent of theory) of the title compound as a bright yellow powder melting at 168°-169° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux
  3. temperatureAfter 30 min the reaction mixture was cooled
  4. filtrationfiltered
  5. customcollecting the insoluble materials
  6. concentrationThe filtrate was concentrated by evaporation under reduced pressure
  7. customthe residue obtained as well as the insoluble materials
  8. filtrationfrom the filtration
  9. additionwere diluted with water
  10. filtrationThe insoluble solids present were collected by filtration
  11. washwashed with water
  12. customdried