Reaktion #4901

Reaktionsgleichung

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

phosphorus pentasulfide

→

2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-thione

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturto reflux for 18 hr
3. 3
   FiltrationThe mixture was filtered
4. 4
   Extraktionthe filtrate was extracted with dilute sodium hydroxide
5. 5
   EinengenThe chloroform layer was concentrated
6. 6
   workup.DISSOLUTIONthe residue was dissolved in 250 ml of boiling isopropyl alcohol
7. 7
   TemperaturOn cooling
8. 8
   Sonstige28 g (44%) of yellow solid precipitated
9. 9
   SonstigeA portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.

Vorschrift

To a solution of 59 g (0.25 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)one hydrochloride in 1500 ml of chloroform was added 41.5 g (0.19 mole) of phosphorus pentasulfide and the mixture was heated to reflux for 18 hr. The mixture was filtered and the filtrate was extracted with dilute sodium hydroxide. The chloroform layer was concentrated and the residue was dissolved in 250 ml of boiling isopropyl alcohol. On cooling, 28 g (44%) of yellow solid precipitated. A portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.

Quelle