تفاعل #4921

معادلة التفاعل

phosphorus pentasulfide

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

phosphorus pentasulfide

→

yellow crystals

المردود 125.6%

2-(2-Chloroethyl)-2,3-dihydro-7-fluoro-4-methyl-1,4-benzoxazepine-5(4H)-thione

المردود 125.6%

المذيبات

toluene

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture heated to reflux
2. 2
   درجة الحرارةheating
3. 3
   workup.WAITcontinued for 2 hr
4. 4
   ترشيحfiltered
5. 5
   غسيلThe filtrate was washed carefully with 3×50 ml of saturated sodium bicarbonate and 50 ml of water
6. 6
   تجفيفdried over sodium sulfate
7. 7
   ترشيحfiltered
8. 8
   ترشيحfiltered
9. 9
   تركيزconcentrated by rotary evaporation
10. 10
    أخرىThe crude material was recrystallized from diisopropyl ether

الإجراء التجريبي

To 1.0 g (0.0039 mole) of 2-(2-chloroethyl)-2,3-dihydro-7-fluoro-4-methyl-1,4-benzoxazepin-5(4H)-one in 30 ml of acetonitrile was added 0.7 g (0.0016 mole) of phosphorus pentasulfide and the reaction mixture heated to reflux. After 2 hr, another 0.4 g (0.009 mole) of phosphorus pentasulfide was added and heating continued for 2 hr. The reaction mixture was diluted with 70 ml of toluene and filtered. The filtrate was washed carefully with 3×50 ml of saturated sodium bicarbonate and 50 ml of water, dried over sodium sulfate, filtered, charcoaled, filtered and concentrated by rotary evaporation. The crude material was recrystallized from diisopropyl ether to give 0.55 g (52%) of yellow crystals, m.p. 135°-137° C.

المصدر