반응 #215149
ord-bc89eb0d2df646f996f9f6665bf9d40e
반응 방정식
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도the mixture heated at 95°-100° C. for about 2 hours
- 2농축The reaction mixture was concentrated under reduced pressure at about 40°-45° C. on a rotary evaporator
- 3workup.ADDITIONThe concentrate was then diluted with approximately 2 volumes of isopropanol
- 4workup.ADDITIONadded slowly to about 600 ml of vigorously stirred water
- 5여과The precipitate was collected by filtration
- 6세척washed with water
- 7기타dried under reduced pressure
실험 절차
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.).