Reaktion #6315

Reaktionsgleichung

5-(methylthio)-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one

isopropylamine

ethanol

ethanol

→

desired product

Ausbeute 62.3%

5-[(1-Methylethyl)amino]-8-[3-(trifluoromethyl)-phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one

Ausbeute 62.3%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture is heated on a steambath for 18 hours
2. 2
   TemperaturThe mixture is cooled to 10° C.
3. 3
   FiltrationThe product is collected by filtration
4. 4
   Waschenwashed with ethanol (2×20 ml)
5. 5
   Sonstigeair-dried

Vorschrift

To a suspension of 5.0 g of 5-(methylthio)-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one in 35 ml of acetic acid is added 2.64 g of isopropylamine. The reaction mixture is heated on a steambath for 18 hours. The resulting solution is cooled to room temperature and 17 ml of ethanol added. The mixture is cooled to 10° C. and 35 ml of ethanol and 20 g of ice added. The mixture is stirred for an additional 30 minutes at -10° C. The product is collected by filtration, washed with ethanol (2×20 ml) and air-dried to give 3.2 g (62.3%) of the desired product.

Quelle