Reacción #3876

Ecuación de reacción

3-[2-[4-(4-trifluoromethylphenoxy)phenoxy]-propionyl]-thiocarbazic acid-O-ethyl ester

→

compound

Rendimiento 57.4%

2-ethoxy-5-[1-[4-(4-trifluoromethylphenoxy)phenoxy]-ethyl]-1,3,4-thiadiazole

Rendimiento 57.4%

Disolventes

sulfuric acid

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGAfter stirring at the same temperature for 10 minutes
3. 3
   Extracciónby extracting with ethyl acetate
4. 4
   LavadoThe resulting ethyl acetate layer was washed with water
5. 5
   Secadodried over anhydrous sodium sulfate
6. 6
   Concentraciónconcentrated
7. 7
   OtroThe residue was purified by chromatography on silica gel

Procedimiento

To 10 ml of concentrated sulfuric acid cooled to -5° C. was added, with stirring, 2.0 g of 3-[2-[4-(4-trifluoromethylphenoxy)phenoxy]-propionyl]-thiocarbazic acid-O-ethyl ester gradually. After stirring at the same temperature for 10 minutes, the reaction mixture was poured over 100 g of ice followed by extracting with ethyl acetate. The resulting ethyl acetate layer was washed with water, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by chromatography on silica gel to obtain 1.1 g of the compound No. 5 described in Table 1.

Fuente