반응 #334459

반응 방정식

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

용매

toluene

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도at reflux for 24 hr
3. 3
   여과The mixture was filtered hot
4. 4
   농축the filtrate concentrated under reduced pressure
5. 5
   기타Yellow solid, 6.5 g (35%) was obtained which
6. 6
   기타was recrystallized from ethanol, m.p. 166°-168° C.

실험 절차

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.

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