Reaktion #975442

Reaktionsgleichung

hexane

(2-chloroethyl)(phenyl)sulfane

potassium carbonate

2-mercapto-3-nitropyridine

→

3-nitro-2-(2-phenylsulfanyl-ethylsulfanyl)pyridine

Ausbeute 66.0%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONThen the mixture was diluted with EE
2. 2
   Waschenwashed with brine
3. 3
   SonstigeThe organic phase was separated off
4. 4
   Trocknendried over Na2SO4
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated to small volume under vacuum

Vorschrift

3.44 g (20.0 mmol) (2-chloroethyl)(phenyl)sulfane and 5.53 g (40.0 mmol) potassium carbonate were added to a solution of 1.56 g (10.0 mmol) 2-mercapto-3-nitropyridine in DMF (30 ml) and heated for 4 h at 60° C. Then the mixture was diluted with EE and washed with brine. The organic phase was separated off, dried over Na2SO4, filtered and concentrated to small volume under vacuum. Column chromatography (hexane/EE 9:1) of the residue yielded 1.93 g (6.6 mmol, 66%) 3-nitro-2-(2-phenylsulfanyl-ethylsulfanyl)pyridine.

Quelle