Réaction #955912

Équation de réaction

thiosemicarbazide

2,4-dimethylbenzoyl chloride

→

powder

Rendement 43.0%

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

Rendement 43.0%

Solvants

pyridine

Conditions de réaction

Traitement

1. 1
   AutreThe yellow solution was evaporated to dryness
2. 2
   workup.ADDITIONdiluted with water
3. 3
   AutreThe white solid was then collected
4. 4
   Lavagewashed with water
5. 5
   TempératureThe suspension was heated at 180° C. for 1 h
6. 6
   FiltrationThen the mixture was filtered hot
7. 7
   Températurethe aqueous solution was cooled in ice
8. 8
   FiltrationThe solid was filtered
9. 9
   Lavagewashed with water
10. 10
    Autredried

Mode opératoire

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%).

Source