تفاعل #4902

معادلة التفاعل

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

phosphorus pentasulfide

potassium sulfide

→

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

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةat reflux for 24 hr
3. 3
   ترشيحThe mixture was filtered hot
4. 4
   تركيزthe filtrate concentrated under reduced pressure
5. 5
   أخرىYellow solid, 6.5 g (35%) was obtained which
6. 6
   أخرىwas recrystallized from ethanol, m.p. 166°-168° C.

الإجراء التجريبي

To a solution of 16.6 g (0.06 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepin-5(4H)-one in 150 ml of dry toluene was added a mixture of 8.6 g (0.045 mole) of phosphorus pentasulfide and 8.6 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux for 24 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure. Yellow solid, 6.5 g (35%) was obtained which was recrystallized from ethanol, m.p. 166°-168° C.

المصدر