Reaktion #1694240

Reaktionsgleichung

dithiolate

potassium hydroxide

dimedone

carbon disulfide

N-methyl-ethylenediamine

glyoxal-sodium bisulfite

→

2-[2-methyl-2,5-diaza-7,9-dithiabicyclo-(4,3, 0)-nonane-8-ylidene]-5,5-dimethyl-1,3-cyclohexanedione

Lösungsmittel

dimethylsulfoxide

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added dropwise with ice-
2. 2
   workup.ADDITIONThen to this solution was added dropwise with ice-
3. 3
   Sonstigeprepared in the manner

Vorschrift

To a suspension of 5.68 g (0.02 mole) of glyoxal-sodium bisulfite in 30 ml of water was added dropwise with ice-cooling 1.5 g (0.02 mole) of N-methyl-ethylenediamine. Then to this solution was added dropwise with ice-cooling the dithiolate solution prepared in the manner shown below; To mixture of 2.8 g (0.02 mole) of dimedone and 1.6 g (0.021 mole) of carbon disulfide in 20 ml of dimethylsulfoxide was added at room temperature 2.7 g (0.044 mole) of powdered potassium hydroxide and the mixture was stirred for 1 hour.

Quelle