반응 #10862
ord-51889edae8a3452c876a139b2f003a44
반응 방정식
반응 조건
온도
65°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도was cooled
- 2세척washed (water)
- 3건조dried (magnesium sulfate)
- 4기타evaporated
- 5기타separated by chromatography on silica gel
실험 절차
Cupric chloride (0.673 g, 2.5 equivalents) was added in one portion to a solution of 3-(2,6-dichloro-4-trifluoromethylphenylhydrazino)propionitrile (0.591 g, 2 mmol) in chlorobenzene, and the mixture heated at 65° C. for 50 minutes. The reaction was judged to be complete and was cooled, washed (water), dried (magnesium sulfate), evaporated and separated by chromatography on silica gel to give 3-(2,6-dichloro-4-trifluoromethylphenylhydrazono)propionitrile, NMR 3.37 (d, 2H), 7.03 (t, 1H), 7.5 (s, 2H), 7.75 (s, 1H) (35% yield), and 3-(2,6-dichloro-4trifluoromethylphenylazo)propionitrile, NMR 3.0 (t, 2H), 4.6 (t, 2H), 7.6 (s, 2H) (60% yield).