반응 #75381

ord-a14458c8825d4459a0d1cea8d0e9f4b1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe mixture was stirred for one hour at this temperature
  2. 2
    workup.ADDITIONThen, the reaction mixture was poured over ice
  3. 3
    여과the precipitate was suction-filtered off
  4. 4
    세척washed neutral with water
  5. 5
    기타dried in the air
  6. 6
    온도After cooling
  7. 7
    여과the crystals were suction-filtered off
  8. 8
    세척washed with ether

실험 절차

220 gm of 4,4-dimethyl-7-acetamino-2H,4H-isoquinoline-1,3-dione were added in portions to 800 ml of fuming nitric acid at -20° C. while stirring. The mixture was stirred for one hour at this temperature. Then, the reaction mixture was poured over ice, the precipitate was suction-filtered off, washed neutral with water, dried in the air, and boiled with isopropanol. After cooling, the crystals were suction-filtered off and washed with ether, yielding 222 gm (85% of theory) of 4,4-dimethyl-7-acetamino-8-nitro-2H,4H-isoquinoline-1,3-dione, m.p. 249° C. (decomp.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04176184uspto-grants-1979_11