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

HRID 3119

反応式

HRID 3119 の反応式
[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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 10219390chromium (VI) trioxide触媒HCID 176Acetic Acid溶媒HCID 7918Acetic Anhydride溶媒

反応条件

温度
80 °C

実験手順

To a stirred warm (80° C.) solution of 6-iodo-1H-indole-2,3-dione (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).

後処理

  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

出典と根拠

ORDレコード
ord-57ce19bea6534a878ad8a04143464a6c
出典データセット
uspto-grants-1998_03
特許番号
US05733910

関連ノート

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