Reaktion #4920

Reaktionsgleichung

phosphorus pentasulfide

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

phosphorus pentasulfide

→

yellow crystals

Ausbeute 173.5%

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

Ausbeute 173.5%

Lösungsmittel

toluene

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture heated
2. 2
   Temperaturto reflux for 2 hr
3. 3
   Temperaturheating
4. 4
   TemperaturAfter cooling
5. 5
   Filtrationfiltered
6. 6
   WaschenThe filtrate was washed with 3×50 ml of saturated sodium bicarbonate and 100 ml of water
7. 7
   Trocknendried over sodium sulfate
8. 8
   Filtrationfiltered
9. 9
   Filtrationfiltered
10. 10
    Einengenconcentrated by rotary evaporation
11. 11
    SonstigeThe crude oil was crystallized from isopropyl ether/toluene

Vorschrift

To 2.0 g (0.007 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-7-nitro-1,4-benzoxazepin-5(4H)-one in 35 ml of acetonitrile was added 1.0 g (0.0023 mole) of phosphorus pentasulfide and the mixture heated to reflux for 2 hr. Another 0.4 g (0.001 mole) of phosphorus pentasulfide was added and heating continued for 2 hr. After cooling, the reaction mixture was diluted with 100 ml of toluene and filtered. The filtrate was washed with 3×50 ml of saturated sodium bicarbonate and 100 ml of water, dried over sodium sulfate, filtered, charcoaled, filtered, and concentrated by rotary evaporation. The crude oil was crystallized from isopropyl ether/toluene to give 1.2 g (57%) of yellow crystals, m.p. 153°-155° C.

Quelle