HRID67779
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
4.8 g (0.01 mole) of 4-(4-chloro-3-chlorosulfonylphenyl)-3-methyl-2-phenylimino-4-thiazoline hydrobromide are added in portions to a mixture of 5 ml (about 0.05 mole) of 40% strength aqueous dimethylamine solution and 50 ml of methanol (or ethanol), with external cooling and stirring, at a rate such that the temperature as far as possible does not rise above 35° C. The reaction mixture is stirred for 14 hours at room temperature, the solvent is distilled off under a waterpump vacuum and the residue is crystallized under 50 ml of water, stirring with a magnetic stirrer. Colorless crystals; melting point 178°-181° C.
WORKUP
后处理
- temperaturewith external cooling
- customas possible does not rise above 35° C
- stirringThe reaction mixture is stirred for 14 hours at room temperature
- distillationthe solvent is distilled off under a waterpump vacuum
- customthe residue is crystallized under 50 ml of water
- stirringstirring with a magnetic stirrer