반응 #955909

반응 방정식

thiosemicarbazide

2-methoxy-4-methylbenzoic acid

EDCI

→

powder

수율 47.0%

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

수율 47.0%

용매

pyridine

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction was stirred at r.t. for 21 h
2. 2
   기타The mixture was evaporated to dryness
3. 3
   workup.ADDITIONdiluted with water
4. 4
   여과The white solid was then filtered
5. 5
   세척washed with water
6. 6
   온도heated
7. 7
   온도at reflux for 2 days
8. 8
   여과The suspension was filtered hot
9. 9
   온도the aqueous solution was cooled in ice
10. 10
    여과The solid was filtered
11. 11
    세척washed with water
12. 12
    기타dried

실험 절차

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%).

출처