Reaktion #4931

Reaktionsgleichung

isopropyl alcohol

maleic acid

2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)-one hydrochloride

morpholine

sodium hydroxide

→

2,3-Dihydro-4-methyl-2-[2-(4-morpholinyl)ethyl]pyrido[3,2-f][1,4]oxazepin-5(4H)-one maleate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe resulting mixture extracted with chloroform (3×30 ml)
2. 2
   SonstigeThe chloroform was removed on the rotary evaporator with aspiration
3. 3
   SonstigeThe residual morpholine was removed in vacuo at 50° C.
4. 4
   Sonstige(rotary evaporator)
5. 5
   TemperaturThe mixture was heated
6. 6
   Temperaturthe clear solution cooled at 20° C. for several hours
7. 7
   SonstigeThe resulting crystals, 16 g (68.1%), were recrystallized from isopropyl alcohol, m.p. 163°-165° C.

Vorschrift

2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)-one hydrochloride, 16 g (058 mole) was dissolved in morpholine (30 mL) and stirred overnight at room temperature. To the solution was added dilute sodium hydroxide solution (50 ml) and the resulting mixture extracted with chloroform (3×30 ml). The chloroform was removed on the rotary evaporator with aspiration. The residual morpholine was removed in vacuo at 50° C. (rotary evaporator). To the residual free base (15.5 g, 0.053 mole) was added isopropyl alcohol (1 liter) and maleic acid (9.24 g g, 0.080 mole). The mixture was heated to boiling and the clear solution cooled at 20° C. for several hours. The resulting crystals, 16 g (68.1%), were recrystallized from isopropyl alcohol, m.p. 163°-165° C.

Quelle