반응 #955912

반응 방정식

thiosemicarbazide

2,4-dimethylbenzoyl chloride

→

powder

수율 43.0%

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

수율 43.0%

용매

pyridine

반응 조건

후처리

1. 1
   기타The yellow solution was evaporated to dryness
2. 2
   workup.ADDITIONdiluted with water
3. 3
   기타The white solid was then collected
4. 4
   세척washed with water
5. 5
   온도The suspension was heated at 180° C. for 1 h
6. 6
   여과Then the mixture was filtered hot
7. 7
   온도the aqueous solution was cooled in ice
8. 8
   여과The solid was filtered
9. 9
   세척washed with water
10. 10
    기타dried

실험 절차

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%).

출처