Acetic Acid → 3,7-Dichloro-1,2,4-benzotriazine

HRID 1834022ノート

反応式

HRID 1834022 の反応式
[Cl:1][C:2]1[N:3]=[N+:4]([O-])[C:5]2[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:6]=2[N:7]=1.[Cl-].[NH4+].C(O)(=O)C>O.[Zn]>[Cl:1][C:2]1[N:3]=[N:4][C:5]2[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:6]=2[N:7]=1

参加物

6

反応物 3

HCID 176Acetic AcidHCID 25517Ammonium ChlorideHCID 130939893,7-Dichloro-1-oxo-1lambda~5~,2,4-benzotriazine

生成物 1

HCID 205554783,7-Dichloro-1,2,4-benzotriazine

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 962Water溶媒

実験手順

A suspension of 21,8 g (0.1 mole) of 3,7-dichlorobenzo-1,2,4-triazine 1-oxide, 7.5 g of zinc dust and 5.5 g of ammonium chloride in 400 ml of water was stirred vigorously at room temperature for 24 hours. 50 ml of glacial acetic acid were then added, the mixture was stirred for a further hour and the insoluble constituents were then filtered off. The latter were extracted twice with methylene chloride. The combined methylene chloride solutions were washed with water, dried over sodium sulfate and evaporated in vacuo. The residue was recrystallized from wash benzine. 7.5 g, that is to say 37% of theory, of 3,7-dichloro-benzo-1,2,4-triazine with a melting point of 113°-115° C were obtained. ##STR36## (Preparation according to process variant (a))

後処理

  1. stirringthe mixture was stirred for a further hour
  2. filtrationthe insoluble constituents were then filtered off
  3. extractionThe latter were extracted twice with methylene chloride
  4. washThe combined methylene chloride solutions were washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo
  7. customThe residue was recrystallized
  8. washfrom wash benzine

出典と根拠

ORDレコード
ord-bafbf11dfefe4b6b83c049bf0034251e
出典データセット
uspto-grants-1978_01
特許番号
US04067981

反応ノート

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