Water → 5,7-Dimethyl-2H-3,1-benzoxazine-2,4(1H)-dione

HRID 3109

반응식

HRID 3109 반응식
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[C:7]2[C:3]=1[C:4](=[O:13])[C:5](=[O:12])[NH:6]2.[OH2:14]>C(O)(=O)C.[O-2].[O-2].[O-2].[Cr+6]>[CH3:1][C:2]1[C:3]2[C:4](=[O:13])[O:12][C:5](=[O:14])[NH:6][C:7]=2[CH:8]=[C:9]([CH3:11])[CH:10]=1

참가 물질

5

반응물 2

HCID 962WaterHCID 23861614,6-dimethyl-1H-indole-2,3-dione

생성물 1

HCID 189298545,7-Dimethyl-2H-3,1-benzoxazine-2,4(1H)-dione수율 31%

시약·촉매·용매 2

HCID 10219390chromium (VI) trioxide촉매HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

To a stirred warm (60° C.) solution of 4,6-dimethyl-1H-indole-2,3-dione (2.0 g, 11.4 mM) in acetic acid (20 mL) was added in small portions chromium trioxide (6.6 g, 66 mM) while maintaining the temperature of the reaction mixture at 65°-70° C. The reaction mixture was then heated at 80° C. for one hour, cooled, poured into water (150 mL) and filtered to obtain the the title compound (0.67 g, 31%) as a light yellow solid; MS(CI): 192 (M+H).

후처리

  1. temperaturewhile maintaining the temperature of the reaction mixture at 65°-70° C
  2. temperaturecooled
  3. filtrationfiltered

출처 및 근거

ORD 기록
ord-ed246c15161e44ccb5ed8c113f70f2e4
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733910

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