Reaktion #49740

Reaktionsgleichung

t-butyl nitrite

3-amino-4-bromobenzotrifluoride

t-Butyl nitrite

3-amino-4-bromobenzotrifluoride

dimethyl disulphide

→

4-bromo-3-(methylsulphenyl)benzotrifluoride

Lösungsmittel

chloroform

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was warmed until reaction
2. 2
   Waschenwashed with water, hydrochloric acid (2M), water
3. 3
   Trocknendried (MgSO4)
4. 4
   Filtrationfiltered
5. 5
   SonstigeThe filtrate was evaporated to dryness
6. 6
   workup.DISTILLATIONthe residue was distilled

Vorschrift

t-Butyl nitrite (3 ml) was added to a mixture of 3-amino-4-bromobenzotrifluoride (4 g) and dimethyl disulphide (15 ml) in chloroform. The mixture was warmed until reaction started when t-butyl nitrite (11 ml) and a solution of 3-amino-4-bromobenzotrifluoride (16 g) in chloroform were added simultaneously. The resultant mixture was stirred for 24 hours, washed with water, hydrochloric acid (2M), water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 4-bromo-3-(methylsulphenyl)benzotrifluoride (16.4 g) as a yellow oil, b.p. 84°-88° C. at 2 mm Hg.

Quelle