Reaktion #1604376

Reaktionsgleichung

1-(4-amino-3-nitrophenyl)-2-bromopropan-1-one

O-ethyl hydrazinecarbothioate

→

5-(4-amino-3-nitrophenyl)-6-methyl-3,6-dihydro-2H-1,3,4-thiadiazin-2-one

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturare refluxed for 4 hours
2. 2
   TemperaturThe reaction mixture is cooled
3. 3
   FiltrationThe crystalline solid is filtered off
4. 4
   Waschenwashed with cold acetonitrile
5. 5
   Sonstigeto give
6. 6
   Sonstigeafter drying

Vorschrift

36.5 g (134 mM) of 1-(4-amino-3-nitrophenyl)-2-bromopropan-1-one and 24.3 g (202.5 mM) of O-ethyl hydrazinecarbothioate dissolved in 190 ml of acetonitrile are refluxed for 4 hours with stirring. The reaction mixture is cooled and maintained at 0° C. for 16 hours. The crystalline solid is filtered off and washed with cold acetonitrile to give, after drying, 10.4 g of 5-(4-amino-3-nitrophenyl)-6-methyl-3,6-dihydro-2H-1,3,4-thiadiazin-2-one in the form of a solid.

Quelle