반응 #43305

반응 방정식

4-amino-3-mercapto-5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazole

3H-benzo[d]imidazole-5-carboxylic acid

→

title compound

수율 17.5%

6-(1H-Benzo[d]imidazol-6-yl)-3-(3,4,5-trimethoxyphenyl)-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazole

수율 17.5%

용매

phosphoryl chloride

반응 조건

후처리

1. 1
   온도was refluxed for 3 h
2. 2
   기타The solvent was evaporated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane (20 mL)
4. 4
   건조The organic layer was dried over sodium sulfate
5. 5
   농축concentrated

실험 절차

A mixture of 4-amino-3-mercapto-5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazole (80 mg, 0.28 mmol) and 3H-benzo[d]imidazole-5-carboxylic acid (46 mg, 0.28 mmol) in phosphoryl chloride (2 mL) was refluxed for 3 h. The solvent was evaporated and the residue was dissolved in dichloromethane (20 mL). It was neutralized with aqueous sodium carbonate. The organic layer was dried over sodium sulfate, concentrated to give 20 mg (17%) of the title compound as a solid. 1H NMR (CD3OD): 8.55 (s, 1H), 8.35 (s, 1H), 8.01-7.85 (m, 2H), 7.72 (s, 1H), 3.99 (s, 6H), 3.87 (s, 3H).

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