反应 #955909

反应方程式

thiosemicarbazide

2-methoxy-4-methylbenzoic acid

EDCI

→

powder

收率 47.0%

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

收率 47.0%

溶剂

pyridine

反应条件

后处理

1. 1
   workup.STIRRINGthe reaction was stirred at r.t. for 21 h
2. 2
   其他The mixture was evaporated to dryness
3. 3
   workup.ADDITIONdiluted with water
4. 4
   过滤The white solid was then filtered
5. 5
   洗涤washed with water
6. 6
   温度heated
7. 7
   温度at reflux for 2 days
8. 8
   过滤The suspension was filtered hot
9. 9
   温度the aqueous solution was cooled in ice
10. 10
    过滤The solid was filtered
11. 11
    洗涤washed with water
12. 12
    其他dried

实验过程

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%).

来源