HRID127967
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
1-Phenyl-2-(3-sulfamoyl-4-chlorobenzoyl)-hydrazine 5 g (0.015 mol) was dissolved in dimethylformamide (20 ml). To this was added propargyl bromide 3.6 g (0.03 mol) and the mixture heated at 95°-100° C. for about 2 hours. The reaction mixture was concentrated under reduced pressure at about 40°-45° C. on a rotary evaporator. The concentrate was then diluted with approximately 2 volumes of isopropanol and added slowly to about 600 ml of vigorously stirred water. The precipitate was collected by filtration, washed with water and dried under reduced pressure to provide 1-phenyl-1-propynyl-2-(3-sulphamoyl-4-chlorobenzoyl)-hydrazine (m.p. 168°-170° C.).
WORKUP
后处理
- temperaturethe mixture heated at 95°-100° C. for about 2 hours
- concentrationThe reaction mixture was concentrated under reduced pressure at about 40°-45° C. on a rotary evaporator
- additionThe concentrate was then diluted with approximately 2 volumes of isopropanol
- additionadded slowly to about 600 ml of vigorously stirred water
- filtrationThe precipitate was collected by filtration
- washwashed with water
- customdried under reduced pressure