Reaktion #50010

Reaktionsgleichung

2,4-dichloro-6-fluoro-7-[N-(2,2-dimethylpropanoyl)hydrazino]benzothiazole

phosgene

toluene

→

3-(2,4-dichloro-6-fluorobenzothiazol-7-yl)-5-(1,1-dimethylethyl)-1,3,4-oxadiazol-2(3H)-one

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   Sonstigethe toluene was removed in vacuo
3. 3
   Trocknendried over magnesium sulfate
4. 4
   Einengenconcentrated
5. 5
   SonstigeThe residue was recrystallised from isopropanol/diisopropyl ether

Vorschrift

A solution of 1,4 g 2,4-dichloro-6-fluoro-7-[N-(2,2-dimethylpropanoyl)hydrazino]benzothiazole in 8 ml of a 20% solution of phosgene in toluene was heated for 8 hours at 100° C. After cooling, the toluene was removed in vacuo and the residue taken up in dichloromethane. The extract was shaken with aqueous sodium hydrogen carbonate and water, dried over magnesium sulfate and concentrated. The residue was recrystallised from isopropanol/diisopropyl ether. Yield: 0.5 g=40% of theory. m.p.: 157°-158° C.

Quelle