Реакция #975442

Уравнение реакции

hexane

(2-chloroethyl)(phenyl)sulfane

potassium carbonate

2-mercapto-3-nitropyridine

→

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

Выход 66.0%

Растворители

DMF

Условия реакции

Обработка

1. 1
   workup.ADDITIONThen the mixture was diluted with EE
2. 2
   Промывкаwashed with brine
3. 3
   ДругоеThe organic phase was separated off
4. 4
   Сушкаdried over Na2SO4
5. 5
   Фильтрацияfiltered
6. 6
   Концентрированиеconcentrated to small volume under vacuum

Методика

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.

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