Reacción #348195

Ecuación de reacción

5,6-DIHYDRO-5-OXOPYRIDO[2,3-B][1,5]BENZOTHIAZEPINE

OXYCHLORIDE

PHOSPHORUS PENTACHLORIDE

→

5-Chloropyrido[2,3-b][1,5]benzothiazepine

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe reaction mixture is heated
2. 2
   Temperaturaunder reflux for 4 hours
3. 3
   workup.DISTILLATIONthe excess phosphorus oxychloride is eliminated by distillation
4. 4
   LavadoThe organic solution is washed several times with iced water
5. 5
   Secadodried over magnesium sulphate
6. 6
   workup.DISTILLATIONThe solvents are eliminated by distillation under vacuum at ambient temperature
7. 7
   Lavadowashed several times with cold ether
8. 8
   SecadoAfter drying under vacuum, 37 g 5-chloropyrido[2,3-b][1,5]benzothiazepine
9. 9
   Otroare obtained

Procedimiento

40 G 5,6-DIHYDRO-5-OXOPYRIDO[2,3-B][1,5]BENZOTHIAZEPINE ARE ADDED TO A MIXTURE OF 200 CM3PHOSPHORUS OXYCHLORIDE AND 71 G PHOSPHORUS PENTACHLORIDE. The reaction mixture is heated under reflux for 4 hours, then the excess phosphorus oxychloride is eliminated by distillation. The residue is then taken up in 300 cm3 cold chloroform. The organic solution is washed several times with iced water, then dried over magnesium sulphate. The solvents are eliminated by distillation under vacuum at ambient temperature. The residue is taken up in anhydrous ether, then washed several times with cold ether. After drying under vacuum, 37 g 5-chloropyrido[2,3-b][1,5]benzothiazepine are obtained, having a melting point of 134°-135° C.

Fuente