Reaktion #955912

Reaktionsgleichung

thiosemicarbazide

2,4-dimethylbenzoyl chloride

→

powder

Ausbeute 43.0%

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

Ausbeute 43.0%

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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%).

Quelle