反应 #955912

反应方程式

thiosemicarbazide

2,4-dimethylbenzoyl chloride

→

powder

收率 43.0%

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

收率 43.0%

溶剂

pyridine

反应条件

后处理

1. 1
   其他The yellow solution was evaporated to dryness
2. 2
   workup.ADDITIONdiluted with water
3. 3
   其他The white solid was then collected
4. 4
   洗涤washed with water
5. 5
   温度The suspension was heated at 180° C. for 1 h
6. 6
   过滤Then the mixture was filtered hot
7. 7
   温度the aqueous solution was cooled in ice
8. 8
   过滤The solid was filtered
9. 9
   洗涤washed with water
10. 10
    其他dried

实验过程

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%).

来源