Reacción #2358485

Ecuación de reacción

2-fluoro-5-(trifluoromethyl)benzaldehyde

methyl thioglycolate

potassium carbonate

DMF

→

methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate

Rendimiento 93.0%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturathe reaction mixture was cooled to room temperature
2. 2
   Extracciónextracted with tert-butyl methyl ether 3 times
3. 3
   LavadoThe combined organic layer was washed with water
4. 4
   SecadoThe mixture was dried over magnesium sulfate
5. 5
   Concentraciónconcentrated under reduced pressure
6. 6
   OtroThe residue was recrystallized from methanol

Procedimiento

A mixture of 5.0 g of 2-fluoro-5-(trifluoromethyl)benzaldehyde, 3.3 g of methyl thioglycolate, 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60° C. for 2 hours, and then the reaction mixture was cooled to room temperature. To the reaction mixture was added water, and extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with water, followed by saturated aqueous sodium chloride solution. The mixture was dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was recrystallized from methanol to obtain 6.3 g of methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (the present compound 1).

Fuente