반응 #3199

ord-62f911c33ec34c2dbe633593e1d5ee82

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    여과filtered
  3. 3
    기타to separate the precipitated solids
  4. 4
    세척The solids were washed thoroughly with water
  5. 5
    기타dried

실험 절차

To a stirred solution of 4,6-dichloro-1H-indole-2,3-dione (5.00 g, 23.2 mM) in acetic acid (21 mL) and acetic anhydride (21 mL) at 80° C. was added in small portions chromium trioxide (4.12 g, 41.3 mM). The temperature of the reaction mixture was maintained between 80°-90° C. during the addition of the chromium trioxide. After the addition was complete, the reaction mixture was diluted with water (100 mL) and then filtered to separate the precipitated solids. The solids were washed thoroughly with water and then dried to obtain the title compound as a yellow solid (4.13 g, 72%); MS(CI): 232 (M+H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733910uspto-grants-1998_03