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

HRID 3109ノート

反応式

HRID 3109 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 10219390chromium (VI) trioxide触媒HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-ed246c15161e44ccb5ed8c113f70f2e4
出典データセット
uspto-grants-1998_03
特許番号
US05733910

反応ノート

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