تفاعل #4931

معادلة التفاعل

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

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر