Water → 5,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione

HRID 569807

反応式

HRID 569807 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]([Cl: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]>[Cl: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]([Cl:11])[CH:10]=1

参加物

5

反応物 2

HCID 962WaterHCID 2519084,6-Dichloroisatin

生成物 1

HCID 123632155,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione

試薬・触媒・溶媒 2

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

実験手順

To a suspension of 4,6-dichloroindolin-2,3-dione (5.95 g) in acetic acid (95 ml) was added chromium trioxide (16 g) over a period of 15 minutes at 60° C. with stirring and the mixture was stirred at 70°-75° C. for 1 hour. After cooling, the reaction mixture was poured into water (360 ml) and the resulting precipitates were collected by filtration. The filtrate was extracted with ethyl acetate. The extract was washed with water and dried. Removal of the solvent gave a residue, which was combined with the precipitates. Recrystallization from isopropyl ether gave 5,7-dichloro-2H-3,1-benzoxazine-2,4(1H)-dione (2.85 g).

後処理

  1. stirringthe mixture was stirred at 70°-75° C. for 1 hour
  2. temperatureAfter cooling
  3. customthe resulting precipitates
  4. filtrationwere collected by filtration
  5. extractionThe filtrate was extracted with ethyl acetate
  6. washThe extract was washed with water
  7. customdried
  8. customRemoval of the solvent
  9. customgave a residue, which
  10. customRecrystallization from isopropyl ether

出典と根拠

ORDレコード
ord-96b79913e52e4204b7065cc2cf9372a3
出典データセット
uspto-grants-1988_03
特許番号
US04734419

関連ノート

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