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
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
A mixture of 0.38 g of 4-ethoxybenzylamine hydrochloride, 0.4 g of 4,5-dibromo-2-iso-propyl-3(2H)pyridazinone, 0.34 g of potassium carbonate, 6 ml of 1,4-dioxane and 18 ml of water, was heated at 90° C. under stirring for 10 hours. The sovent was distilled off under reduced pressure, and water was added to the residue thereby obtained, and the mixture was extracted with ethyl acetate. The extract was washed with diluted hydrochloric acid and a saturated sodium chloride aqueous solution, and dried over sodium sulfate, and then the solvent was distilled off. The product was crystallized from ether to obtain 220 mg of the above identified compound having a melting point of from 151° to 152.5° C. as pale yellow crystals.
WORKUP
后处理
- distillationThe sovent was distilled off under reduced pressure, and water
- additionwas added to the residue
- customthereby obtained
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with diluted hydrochloric acid
- dry with materiala saturated sodium chloride aqueous solution, and dried over sodium sulfate
- distillationthe solvent was distilled off
- customThe product was crystallized from ether
- customto obtain 220 mg of the
- customof from 151° to 152.5° C.