Reaktion #63461

Reaktionsgleichung

6-(3,4-Dihydro-1,4(2H)-benzoxazin-6-yl)-2,3,4,5-tetrahydropyridazin-3-one

triethylamine

3,4-dimethoxybenzoylchloride

→

6-(3,4-Dihydro-4-(3,4-dimethoxyphenylcarbonyl)-1,4(2H)-benzoxazin-6-yl)-2,3,4,5-tetrahydropyridazin-3-one

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture heated
2. 2
   Temperaturat reflux for four hours
3. 3
   WaschenThe solution was washed with sodium bicarbonate solution
4. 4
   Sonstigeevaporated to dryness
5. 5
   SonstigeThe residue was chromatographed on silica gel eluting with 1:1 ethyl acetate
6. 6
   SonstigeThe title compound was collected as white needles, mp 207°-208° C.

Vorschrift

6-(3,4-Dihydro-1,4(2H)-benzoxazin-6-yl)-2,3,4,5-tetrahydropyridazin-3-one was dissolved in methylene chloride and 1.1 equivalent of triethylamine. 1.1 equivalent of 3,4-dimethoxybenzoylchloride was added and the mixture heated at reflux for four hours. The solution was washed with sodium bicarbonate solution and then evaporated to dryness. The residue was chromatographed on silica gel eluting with 1:1 ethyl acetate:ethyl ether. The title compound was collected as white needles, mp 207°-208° C.

Quelle