تفاعل #955909

معادلة التفاعل

thiosemicarbazide

2-methoxy-4-methylbenzoic acid

EDCI

→

powder

المردود 47.0%

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

المردود 47.0%

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe reaction was stirred at r.t. for 21 h
2. 2
   أخرىThe mixture was evaporated to dryness
3. 3
   workup.ADDITIONdiluted with water
4. 4
   ترشيحThe white solid was then filtered
5. 5
   غسيلwashed with water
6. 6
   درجة الحرارةheated
7. 7
   درجة الحرارةat reflux for 2 days
8. 8
   ترشيحThe suspension was filtered hot
9. 9
   درجة الحرارةthe aqueous solution was cooled in ice
10. 10
    ترشيحThe solid was filtered
11. 11
    غسيلwashed with water
12. 12
    أخرىdried

الإجراء التجريبي

To a solution of 2-methoxy-4-methylbenzoic acid (1.81 g, 9.22 mmol) in 9 ml of pyridine was added EDCI (1.9 g, 9.3 mmol) and the suspension was stirred at r.t. for 1 h. Then thiosemicarbazide (800 mg, 8.8 mmol) was added and the reaction was stirred at r.t. for 21 h. The mixture was evaporated to dryness and then diluted with water. The white solid was then filtered, washed with water and suspended in 20 ml 1 M aq. NaHCO3 and then heated at reflux for 2 days. The suspension 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 a white powder (47%).

المصدر