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
To 51 g (0.315 mole) of 2,6-dichloroaniline is added 0.4 moles of ethereal HCl and 200 ml of m-cresol. The mixture is then sitrred and heated on a steam bath to drive off the ether and excess hydrogen chloride. To the resultant mixture is then added 17.7 g (0.315 mole) of methyl cyanamide then heated for 2 hours on a steam bath. The reaction mixture is then cooled, added to 150 ml of conc. sodium hydroxide solution, cooled and extracted with 2 liters of ether. The ether layer is washed with 2×1 liter of water, dried over sodium sulfate, charcoaled and evaporated. The residue is triturated with hexane and the precipitate is filtered off and washed with ether and dried to obtain 1-(2,6-dichlorophenyl)-3-methylguanidine hydrochloride.
WORKUP
后处理
- temperatureheated on a steam bath
- temperaturethen heated for 2 hours on a steam bath
- temperatureThe reaction mixture is then cooled
- temperaturecooled
- extractionextracted with 2 liters of ether
- washThe ether layer is washed with 2×1 liter of water
- dry with materialdried over sodium sulfate
- customevaporated
- customThe residue is triturated with hexane
- filtrationthe precipitate is filtered off
- washwashed with ether
- customdried