HRID127967

反应详情

EQUATION

反应方程式

HRID 127967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture heated at 95°-100° C. for about 2 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure at about 40°-45° C. on a rotary evaporator
  3. additionThe concentrate was then diluted with approximately 2 volumes of isopropanol
  4. additionadded slowly to about 600 ml of vigorously stirred water
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with water
  7. customdried under reduced pressure