Water → HCID 21286378, Verbindung

HRID 2231188Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2231188
[Cl:1][C:2]1[CH:3]=[C:4]([N:20]2[C:25](=[O:26])[NH:24][C:23](=[O:27])[CH2:22][NH:21]2)[CH:5]=[C:6]([Cl:19])[C:7]=1[O:8][C:9]1[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:11][CH:10]=1.S(=O)(=O)(O)O.O.[C:34](OC(=O)C)(=[O:36])[CH3:35]>>[C:34]([N:21]1[CH2:22][C:23](=[O:27])[NH:24][C:25](=[O:26])[N:20]1[C:4]1[CH:5]=[C:6]([Cl:19])[C:7]([O:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:13][CH:14]=2)=[C:2]([Cl:1])[CH:3]=1)(=[O:36])[CH3:35]

Komponenten

5

Edukt 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 13823230HCID 13823230, Verbindung

Produkt 1

HCID 21286378HCID 21286378, Verbindung

Versuchsvorschrift

2 g of 2-[3,5-dichloro-4-(4-methylsulfonylphenoxy)phenyl]hexahydro-1,2,4-triazine-3,5-dione were suspended in 10 ml of acetic anhydride. 1 ml of concentrated sulfuric acid was added dropwise, during which there was a slight increase in the temperature of the suspension and the starting material slowly dissolved. The mixture was then stirred at room temperature for 2 to 3 hours, and was subsequently stirred with water. The product was filtered off with suction, washed with water and dried, and recrystallized from a little glacial acetic acid, melting point 267° C.

Aufarbeitung

  1. temperaturea slight increase in the temperature of the suspension
  2. dissolutionthe starting material slowly dissolved
  3. filtrationThe product was filtered off with suction
  4. washwashed with water
  5. customdried
  6. customrecrystallized from a little glacial acetic acid, melting point 267° C.

Quellen und Nachweise

ORD-Eintrag
ord-0b1688980ddd43378d5fa808086afb80
Quelldatensatz
uspto-grants-1988_11
Patentnummer
US04782056

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