반응 #4900

반응 방정식

phosphorus pentasulfide

potassium sulfide

2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one

→

2-(2-Chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione

용매

toluene

반응 조건

후처리

1. 1
   온도the mixture refluxed 24 hr
2. 2
   여과and filtered
3. 3
   농축The filtrate was concentrated
4. 4
   기타partitioned between chloroform and diluted sodium hydroxide
5. 5
   농축The chloroform layer was concentrated
6. 6
   기타the residue was crystallized several times from ethanol

실험 절차

A mixture of 18.5 g (0.0834 mole) of phosphorus pentasulfide and 18.5 g potassium sulfide was ground together and added to a solution of 100 g (0.417 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in dry toluene, the mixture refluxed 24 hr. and filtered. The filtrate was concentrated and partitioned between chloroform and diluted sodium hydroxide. The chloroform layer was concentrated and the residue was crystallized several times from ethanol. Yield of product was 55 g (52%), m.p. 105°-108° C.

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