تفاعل #4901

معادلة التفاعل

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

المذيبات

chloroform

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةto reflux for 18 hr
3. 3
   ترشيحThe mixture was filtered
4. 4
   استخلاصthe filtrate was extracted with dilute sodium hydroxide
5. 5
   تركيزThe chloroform layer was concentrated
6. 6
   workup.DISSOLUTIONthe residue was dissolved in 250 ml of boiling isopropyl alcohol
7. 7
   درجة الحرارةOn cooling
8. 8
   أخرى28 g (44%) of yellow solid precipitated
9. 9
   أخرىA portion was recrystallized from isopropyl alcohol, m.p. 134°-136° C.

الإجراء التجريبي

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.

المصدر