Реакция #955912

Уравнение реакции

thiosemicarbazide

2,4-dimethylbenzoyl chloride

→

powder

Выход 43.0%

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

Выход 43.0%

Растворители

pyridine

Условия реакции

Обработка

1. 1
   ДругоеThe yellow solution was evaporated to dryness
2. 2
   workup.ADDITIONdiluted with water
3. 3
   ДругоеThe white solid was then collected
4. 4
   Промывкаwashed with water
5. 5
   ТемператураThe suspension was heated at 180° C. for 1 h
6. 6
   ФильтрацияThen the mixture was filtered hot
7. 7
   Температураthe aqueous solution was cooled in ice
8. 8
   ФильтрацияThe solid was filtered
9. 9
   Промывкаwashed with water
10. 10
    Другоеdried

Методика

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%).

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