Water → 7-Iodo-1H-benzo[d][1,3]oxazine-2,4-dione

HRID 1449567

반응식

HRID 1449567 반응식
[I:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6](=[O:12])[C:7](=[O:11])[NH:8]2)=[CH:4][CH:3]=1.[OH2:13]>C(O)(=O)C.C(OC(=O)C)(=O)C.[O-2].[O-2].[O-2].[Cr+6]>[I:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:12])[O:11][C:7](=[O:13])[NH:8][C:9]=2[CH:10]=1

참가 물질

6

반응물 2

HCID 962WaterHCID 143872746-iodo-2,3-dihydro-1H-indole-2,3-dione

생성물 1

HCID 189299207-Iodo-1H-benzo[d][1,3]oxazine-2,4-dione수율 81.8%

시약·촉매·용매 3

HCID 10219390chromium (VI) trioxide촉매HCID 176Acetic Acid용매HCID 7918Acetic Anhydride용매

반응 조건

온도
80 °C

실험 절차

To a stirred warm (80° C.) solution of 6-iodo-1H-indole-2,3dione (3.0 g, 11 mM) in acetic acid (10 mL) and acetic anhydride (10 mL) was added in small portions chromium trioxide (1.83 g, 18.3 mM) while maintaining the temperature of the reaction mixture at 80°-90° C. The reaction mixture was then heated at 80° C. for 10 min, cooled and poured into water. The resulting mixture was filtered and the collected solids dried to provide the title compound as a yellow solid (2.6 g, 81.8%); MS(CI): 290 (M+H).

후처리

  1. temperaturewhile maintaining the temperature of the reaction mixture at 80°-90° C
  2. temperaturecooled
  3. filtrationThe resulting mixture was filtered
  4. customthe collected solids dried

출처 및 근거

ORD 기록
ord-538c5ab905094dd6a93d5d5fdc38ecb0
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599814

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