반응 #5025

ord-431b0132d8ae40649c3dfbbbb5dc0995

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGAfter stirred at the temperature as such for 7.5 hours
  2. 2
    여과The deposited crystal was collected by filtration
  3. 3
    세척washed with water and acetone
  4. 4
    기타dried

실험 절차

To a mixed solution of acetic acid (3.8 ml), concentrated sulfuric acid (4.7 ml) and funing nitric acid (0.8 ml), under cooling with stirring, were added only small portions of N-acetyl-7-cyano-indoline (2.42 g). After stirred at the temperature as such for 7.5 hours, the reaction mixture was poured into ice-water (50 ml). The deposited crystal was collected by filtration, washed with water and acetone, and then dried to give the intended compound 2.6 g (66.7%) as white powder. M.P.: 245°-255° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05242912uspto-grants-1993_09