反応 #955912

反応方程式

thiosemicarbazide

2,4-dimethylbenzoyl chloride

→

powder

収率 43.0%

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

収率 43.0%

溶媒

pyridine

反応条件

後処理

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

実験手順

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%).

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