HRID255892
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
39.2 g of p-chlorothiobenzoic acid hydrazide are dissolved in 350 ml of ethanol. Under nitrogen, 21.4 g of pyridine-3-aldehyde (dissolved in 20 ml of ethanol) are added dropwise to this solution. The reaction temperature is kept at 20° C. by cooling. When the addition is complete, the reaction mixture is stirred for 1 hour at reflux temperature and subsequently filtered through finely particulate diatomaceous earth. The filtrate is concentrated to three quarters of its initial volume and the precipitated product is isolated by filtration, washed with hexane and dried, affording the title compound of the formula ##STR8## with a melting point of 106°-108° C. (compound 1.1).
WORKUP
后处理
- customis kept at 20° C.
- temperatureby cooling
- additionWhen the addition
- temperatureat reflux temperature
- filtrationsubsequently filtered through finely particulate diatomaceous earth
- concentrationThe filtrate is concentrated to three quarters of its initial volume
- customthe precipitated product is isolated by filtration
- washwashed with hexane
- customdried