Reaktion #49687

Reaktionsgleichung

2-benzylidenehydrazono-3-ethoxycarbonylmethyl-1-methoxycarbonylmethylimidazolidin-4-one

→

7-ethoxycarbonylmethyl-1,4,5,7-tetraazabicyclo[4,3,0]-nonan-5-ene-3,8-dione

Ausbeute 39.1%

Lösungsmittel

hydrochloric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONthe mixture was subjected to a steam distillation for 40 minutes
2. 2
   SonstigeThe reaction mixture obtained
3. 3
   Einengenwas concentrated under reduced pressure
4. 4
   Sonstigethe residue formed
5. 5
   workup.ADDITIONwas charged on silica gel column chromatography
6. 6
   Wascheneluted with a mixture of chloroform and ethyl acetate at 1:2 by volume

Vorschrift

To 230 mg of 2-benzylidenehydrazono-3-ethoxycarbonylmethyl-1-methoxycarbonylmethylimidazolidin-4-one obtained in step (1) of Example 7 was added 10 ml of 0.5N hydrochloric acid, the mixture was subjected to a steam distillation for 40 minutes. The reaction mixture obtained was concentrated under reduced pressure, and the residue formed was charged on silica gel column chromatography and eluted with a mixture of chloroform and ethyl acetate at 1:2 by volume to obtain 60 mg of 7-ethoxycarbonylmethyl-1,4,5,7-tetraazabicyclo[4,3,0]-nonan-5-ene-3,8-dione.

Quelle