Reaktion #1286193

Reaktionsgleichung

triethylamine

2-amino-5-methoxybenzophenone

chlorine

methylthioacetonitrile

→

title product

2-Amino-3-benzoyl-5-methoxy-α-(methylthio)benzeneacetonitrile

Lösungsmittel

methylene chloride

methylene chloride

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile maintaining the temperature below -65° C
2. 2
   workup.ADDITIONis added dropwise over a 30 min period
3. 3
   workup.STIRRINGThe mixture is stirred for about an hour at -70° C.
4. 4
   Temperaturto warm to ambient temperature
5. 5
   WaschenThe mixture is washed with water
6. 6
   Trocknendried over sodium sulfate
7. 7
   Einengenconcentrated under reduced pressure
8. 8
   SonstigeThe residue is recrystallized from a suitable solvent, e.g., 2-propanol

Vorschrift

To a solution of 4.0 ml (0.088 mole) of chlorine in 200 ml of methylene chloride cooled to -70° C. is added dropwise a solution of 7.65 g (0.088 mole) of methylthioacetonitrile in 1 liter of methylene chloride while maintaining the temperature below -65° C. After several minutes a solution containing 0.2 mole of 2-amino-5-methoxybenzophenone in 100 ml of methylene chloride is added dropwise over a 30 min period. The mixture is stirred at -70° C. for about 1.5 hr and 18 g (0.18 mole) of triethylamine is added. The mixture is stirred for about an hour at -70° C. and then allowed to warm to ambient temperature. The mixture is washed with water, dried over sodium sulfate and concentrated under reduced pressure. The residue is recrystallized from a suitable solvent, e.g., 2-propanol, to give the title product.

Quelle