HRID963153
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated
- temperatureto reflux
- temperatureAfter 30 min the reaction mixture was cooled
- filtrationfiltered
- customcollecting the insoluble materials
- concentrationThe filtrate was concentrated by evaporation under reduced pressure
- customthe residue obtained as well as the insoluble materials
- filtrationfrom the filtration
- additionwere diluted with water
- filtrationThe insoluble solids present were collected by filtration
- washwashed with water
- customdried