تفاعل #4904

معادلة التفاعل

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

phosphorus pentasulfide

potassium sulfide

→

yellow solid

المردود 72.6%

7-Bromo-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione

المردود 72.6%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture was heated
2. 2
   درجة الحرارةat reflux for 5 hr under a nitrogen atmosphere
3. 3
   ترشيحThe mixture was filtered hot
4. 4
   تركيزthe filtrate concentrated under reduced pressure
5. 5
   workup.DISSOLUTIONThe residue was dissolved in chloroform
6. 6
   غسيلThe chloroform solution was washed twice with dilute aqueous sodium hydroxide
7. 7
   تجفيفdried over magnesium sulfate
8. 8
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

To a solution of 11.0 g (0.035 mole) of 7-bromo-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in 150 ml of dry toluene was added a mixture of 13.4 g (0.07 mole) of phosphorus pentasulfide and 13.4 g of potassium sulfide which had been ground together. The reaction mixture was heated at reflux for 5 hr under a nitrogen atmosphere. The mixture was filtered hot and the filtrate concentrated under reduced pressure. The residue was dissolved in chloroform. The chloroform solution was washed twice with dilute aqueous sodium hydroxide, dried over magnesium sulfate and concentrated under reduced pressure to give 8.5 g (72%) of yellow solid. The solid was recrystallized from ethanol, m.p. 118°-120° C.

المصدر