Water → 5-Mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

HRID 1730991

Reaktionsgleichung

Reaktionsgleichung von HRID 1730991
[C:1]([C:5]1[CH:6]=[C:7]([C:16]2[C:17](=[S:21])[S:18][S:19][CH:20]=2)[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].[S-:22][S-].[Na+].[Na+].O>CN(C)C=O>[SH:22][C:20]1[S:19][S:18][C:17](=[S:21])[C:16]=1[C:7]1[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[C:10]([OH:11])=[C:9]([C:12]([CH3:14])([CH3:15])[CH3:13])[CH:8]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 89870Sodium disulfideHCID 98408264-(3,5-Di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

Produkt 1

HCID 214946305-Mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

33.8 parts of 4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione and 40 parts of a 2.5 molar solution of sodium disulphide were dissolved in 40 parts of dimethylformamide and warmed at 100°C for 15 minutes. 500 parts of water were then added, the mixture extracted several times with ether to remove any starting material, and then 60 parts of 3N hydrochloric acid solution were added slowly with stirring. The solid was filtered giving 27 parts of 5-mercapto-4-(3,5-di-t-butyl-4-hydroxyphenyl)-1,2-dithiole-3-thione m.p. 182°C which gave the following elemental analysis:

Aufarbeitung

  1. extractionthe mixture extracted several times with ether
  2. customto remove any starting material
  3. addition60 parts of 3N hydrochloric acid solution were added slowly
  4. filtrationThe solid was filtered

Quellen und Nachweise

ORD-Eintrag
ord-d522f66c7c614c52a078c15ec093d75f
Quelldatensatz
uspto-grants-1976_11
Patentnummer
US03994923

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