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

HRID 1834022노트

반응식

HRID 1834022 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 962Water용매

실험 절차

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))

후처리

  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

출처 및 근거

ORD 기록
ord-bafbf11dfefe4b6b83c049bf0034251e
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04067981

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