Trichloromethanesulfenyl chloride → HCID 20356007, Verbindung

HRID 371708

Reaktionsgleichung

Reaktionsgleichung von HRID 371708
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12](=[O:13])[NH:11][NH:10][C:9]2=[O:14])[CH:5]=[CH:6][CH:7]=1.[OH-].[Na+].[Cl:17][C:18]([Cl:22])([Cl:21])[S:19]Cl>O>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:9](=[O:14])[N:10]([S:19][C:18]([Cl:22])([Cl:21])[Cl:17])[N:11]([S:19][C:18]([Cl:22])([Cl:21])[Cl:17])[C:12]2=[O:13])[CH:5]=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 11666Trichloromethanesulfenyl chlorideHCID 14798Sodium HydroxideHCID 12855214-(3-Chlorophenyl)-1,2,4-triazolidine-3,5-dione

Produkt 1

HCID 20356007HCID 20356007, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Versuchsvorschrift

To a solution of 42.2g (0.2 mole) 4-(3-chlorophenyl) urazole in 200 ml water was added a solution of 16g (0.4 mole) sodium hydroxide in 20 ml water. A mixture of 74.4g (0.4 mole) trichloromethylsulfenyl chloride and 3g of an emulsifier solution (as in example 1) in 50 ml water was added dropwise to the above basic solution while keeping the reaction mixture at 0° C. The reactants were mixed so that the reaction mixture was kept at a pH greater than 7. The precipitate that formed was filtered and the filter cake was washed with water. After drying and recrystallizing from cyclohexane there was obtained 70g (69%) 4-(3-chlorophenyl)-1,2-bis-(trichloromethylthio) urazole having a melting point of 153° C.

Aufarbeitung

  1. additionwas added dropwise to the above basic solution
  2. customat 0° C
  3. additionThe reactants were mixed so that the reaction mixture
  4. customThe precipitate that formed
  5. filtrationwas filtered
  6. washthe filter cake was washed with water
  7. customAfter drying
  8. customrecrystallizing from cyclohexane

Quellen und Nachweise

ORD-Eintrag
ord-8e2eb88ab11d40b1a7e10e885feceab1
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04087534

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