تفاعل #955912

معادلة التفاعل

thiosemicarbazide

2,4-dimethylbenzoyl chloride

→

powder

المردود 43.0%

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

المردود 43.0%

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   أخرىThe yellow solution was evaporated to dryness
2. 2
   workup.ADDITIONdiluted with water
3. 3
   أخرىThe white solid was then collected
4. 4
   غسيلwashed with water
5. 5
   درجة الحرارةThe suspension was heated at 180° C. for 1 h
6. 6
   ترشيحThen the mixture was filtered hot
7. 7
   درجة الحرارةthe aqueous solution was cooled in ice
8. 8
   ترشيحThe solid was filtered
9. 9
   غسيلwashed with water
10. 10
    أخرىdried

الإجراء التجريبي

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%).

المصدر