Reaktion #2306234

Reaktionsgleichung

dimethyl (2E)-2-[(azepan-2-ylideneamino)oxy]but-2-enedioate

dimethyl (2Z)-2-[(azepan-2-ylideneamino)oxy]but-2-enedioate

→

Methyl 3-hydroxy-4-oxo-4,6,7,8,9,10-hexahydropyrimido[1,2-a]azepine-2-carboxylate

Lösungsmittel

o-xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed
2. 2
   SonstigeAfter 16 h the solvent was removed under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue, dissolved in ethyl acetate
4. 4
   Extraktionwas extracted with a saturated solution of NaHCO3 in water
5. 5
   Extraktionthe solution was extracted with dichloromethane
6. 6
   TrocknenThe organic phase was dried over sodium sulphate
7. 7
   Einengenconcentrated

Vorschrift

A mixture of dimethyl (2E)-2-[(azepan-2-ylideneamino)oxy]but-2-enedioate and dimethyl (2Z)-2-[(azepan-2-ylideneamino)oxy]but-2-enedioate in ratio 8/1 was dissolved in o-xylene and refluxed. After 16 h the solvent was removed under reduced pressure and the residue, dissolved in ethyl acetate, was extracted with a saturated solution of NaHCO3 in water. The pH of the aqueous phase was adjusted to about 3 adding 6M HCl aq. and the solution was extracted with dichloromethane. The organic phase was dried over sodium sulphate and concentrated.

Quelle