반응 #4905

반응 방정식

phosphorus pentasulfide

potassium sulfide

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

→

yellow crystals

수율 84.1%

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

수율 84.1%

용매

toluene

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도at reflux for 7 hr
3. 3
   여과The hot reaction mixture was filtered
4. 4
   기타the product crystallized from the cooled filtrate
5. 5
   기타Recrystallization from chloroform

실험 절차

A mixture of 9.55 g of phosphorus pentasulfide and 9.5 g of potassium sulfide were ground together and added to a solution of 20.2 g (0.07 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepin-5(4H)-one in 200 ml of dry toluene. The mixture was stirred and heated at reflux for 7 hr. The hot reaction mixture was filtered and the product crystallized from the cooled filtrate. Recrystallization from chloroform gave 18 g (84%) of yellow crystals, m.p. 167°-170° C.

출처