반응 #323360

반응 방정식

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

반응 조건

후처리

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

실험 절차

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.

출처