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

HRID 3103

反応式

HRID 3103 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.C(O)(=[O:16])C>C(OC(=O)C)(=O)C.O.[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:16])[NH:6][C:7]=2[CH:8]=[C:9]([Cl:11])[CH:10]=1

参加物

6

反応物 2

HCID 176Acetic AcidHCID 2519084,6-Dichloroisatin

生成物 1

HCID 123632155,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione収率 72%

試薬・触媒・溶媒 3

HCID 10219390chromium (VI) trioxide触媒2 回HCID 962Water溶媒HCID 7918Acetic Anhydride溶媒

実験手順

To a stirred solution of 4,6-dichloro-1H-indole-2,3-dione (5.00 g, 23.2 mM) in acetic acid (21 mL) and acetic anhydride (21 mL) at 80° C. was added in small portions chromium trioxide (4.12 g, 41.3 mM). The temperature of the reaction mixture was maintained between 80°-90° C. during the addition of the chromium trioxide. After the addition was complete, the reaction mixture was diluted with water (100 mL) and then filtered to separate the precipitated solids. The solids were washed thoroughly with water and then dried to obtain the title compound as a yellow solid (4.13 g, 72%); MS(CI): 232 (M+H).

後処理

  1. additionAfter the addition
  2. filtrationfiltered
  3. customto separate the precipitated solids
  4. washThe solids were washed thoroughly with water
  5. customdried

出典と根拠

ORDレコード
ord-62f911c33ec34c2dbe633593e1d5ee82
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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