Reacción #955912

Ecuación de reacción

thiosemicarbazide

2,4-dimethylbenzoyl chloride

→

powder

Rendimiento 43.0%

5-(2,4 dimethylphenyl)-2H-1,2,4-triazole-3(4H)-thione

Rendimiento 43.0%

Disolventes

pyridine

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe yellow solution was evaporated to dryness
2. 2
   workup.ADDITIONdiluted with water
3. 3
   OtroThe white solid was then collected
4. 4
   Lavadowashed with water
5. 5
   TemperaturaThe suspension was heated at 180° C. for 1 h
6. 6
   FiltraciónThen the mixture was filtered hot
7. 7
   Temperaturathe aqueous solution was cooled in ice
8. 8
   FiltraciónThe solid was filtered
9. 9
   Lavadowashed with water
10. 10
    Otrodried

Procedimiento

A suspension of thiosemicarbazide (800 mg, 8.78 mmol) in 9 mL of pyridine was added 2,4-dimethylbenzoyl chloride (1.68 g, 10 mmol). The reaction was heated at 150° C. for 10 min using a microwave synthesizer. The yellow solution was evaporated to dryness and then diluted with water. The white solid was then collected and washed with water. The solid was suspended in 20 mL of 1 M aq. NaHCO3. The suspension was heated at 180° C. for 1 h using a microwave synthesizer. Then the mixture was filtered hot and the aqueous solution was cooled in ice and acidified to pH 3 with conc. HCl. The solid was filtered and washed with water and dried to give white powder (43%).

Fuente