Thionyl Chloride → 3-Chloroisatoic anhydride

HRID 838992

反応式

HRID 838992 の反応式
C([O:3][C:4]([NH:6][C:7]1[C:8](=[CH:12][CH:13]=[CH:14][C:15]=1[Cl:16])[C:9]([OH:11])=[O:10])=O)C.S(Cl)(Cl)=O>O1CCOCC1>[Cl:16][C:15]1[C:7]2[NH:6][C:4](=[O:3])[O:10][C:9](=[O:11])[C:8]=2[CH:12]=[CH:13][CH:14]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 203255893-Chloro-2-[(ethoxycarbonyl)amino]benzoic acid

生成物 1

HCID 5175353-Chloroisatoic anhydride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

468 gm of N-ethoxycarbonyl-3-chloro-anthranilic acid (m.p. 111°-114° C) were refluxed in 1500 ml of dioxane with 420 ml of thionyl chloride for 3 hours while stirring. Thereafter, the reaction solution was evaporated in vacuo until crystallization started, and then cooled. The precipitate was collected by suction filtration and washed with ether. 8-Chloro-2H-3,1-benzoxazine-2,4(1H)-dione, m.p. 225°-230° C, was obtained.

後処理

  1. customThereafter, the reaction solution was evaporated in vacuo until crystallization
  2. temperaturecooled
  3. filtrationThe precipitate was collected by suction filtration
  4. washwashed with ether

出典と根拠

ORDレコード
ord-eabb9a499dfa4e3fa44b3f4e83befdd6
出典データセット
uspto-grants-1978_06
特許番号
US04093734

関連ノート

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