Reacción #1104977

Ecuación de reacción

benzyltrimethylammonium dichloriodate

potassium carbonate

2,5-dimethylaniline

sodium pyrosulphite

→

2,5-dimethyl-4-iodo-aniline

Disolventes

methanol

dichloromethane

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Filtraciónfiltered
2. 2
   workup.DISTILLATIONthe solvent is distilled off
3. 3
   Extracciónextracted with ether
4. 4
   SecadoThe combined organic extracts are dried over sodium sulphate
5. 5
   Otroevaporated down
6. 6
   OtroThe crude product is triturated with petroleum ether, suction
7. 7
   Filtraciónfiltered
8. 8
   Otrodried

Procedimiento

25.0 g (71.8 mmol) of benzyltrimethylammonium dichloriodate and 12.8 g (92.5 mmol) of potassium carbonate are added to a solution of 8.8 ml of (70.8 mmol) of 2,5-dimethylaniline in 250 ml of methanol and 600 ml of dichloromethane and stirred for 1 hour at ambient temperature. Then the inorganic salts are suction filtered and the solvent is distilled off. The residue is combined with a solution of 13.5 g (70.8 mmol) of sodium pyrosulphite in 640 ml of water and extracted with ether. The combined organic extracts are dried over sodium sulphate and evaporated down. The crude product is triturated with petroleum ether, suction filtered and dried.

Fuente