反应详情

0.41 g of 1H-Imidazole-2-carboxylic acid [2-methoxy-5-(tetrahydro-pyran-4-yl)-phenyl]-amide (1.36 mmol) were taken up in toluene (25.0 ml) and treated with 1.65 g of Lawesson reagent (4.08 mmol). The reaction mixture was heated to reflux for 16 h. After cooling to ambient temperature, water (25 ml) was added and the mixture was extracted 3 times with methylene chloride. The combined organic phases were dried on sodium carbonate, evaporated and the residue was dried under high vacuum to yield 0.179 g of 1H-imidazole-2-carbothioic acid [2-methoxy-5-(tetrahydro-pyran-4-yl)-phenyl]-amide (41%) as a yellow solid; M.p.: 189–190° C.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 16 h
3. extractionthe mixture was extracted 3 times with methylene chloride
4. customThe combined organic phases were dried on sodium carbonate
5. customevaporated
6. customthe residue was dried under high vacuum