تفاعل #4900

معادلة التفاعل

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

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture refluxed 24 hr
2. 2
   ترشيحand filtered
3. 3
   تركيزThe filtrate was concentrated
4. 4
   أخرىpartitioned between chloroform and diluted sodium hydroxide
5. 5
   تركيزThe chloroform layer was concentrated
6. 6
   أخرىthe residue was crystallized several times from ethanol

الإجراء التجريبي

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.

المصدر