반응 #215149

ord-bc89eb0d2df646f996f9f6665bf9d40e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04258059uspto-grants-1981_03