反应详情

温度

85 °C

A solution of methyl 2,3-difluoro-4-hydroxy-5-nitrobenzoate in N,N-dimethylformamide is treated with one molar equivalent of cesium carbonate and warmed to 85° C. for 30 minutes. The stirring mixture is then treated dropwise rapidly with a solution comprised of a slight excess of N,N-dimethylthiocarbamoyl chloride in N,N-dimethylformamide. The reaction mixture is stirred at room temperature for one hour, or may be warmed over a steam bath for one hour. The mixture is then poured into water and extracted with ethyl acetate. The organic phase is washed with 5% aqueous sodium hydroxide, water, and brine, and is then dried with a drying agent like magnesium sulfate of sodium sulfate. The solvent is then removed in vacuo to give a crude product. The compound is purified by ordinary methods such as chromatography or crystallization from an appropriate solvent.

1. additionThe stirring mixture is then treated dropwise rapidly with a solution
2. temperaturemay be warmed over a steam bath for one hour
3. extractionextracted with ethyl acetate
4. washThe organic phase is washed with 5% aqueous sodium hydroxide, water, and brine
5. dry with materialis then dried with a drying agent like magnesium sulfate of sodium sulfate
6. customThe solvent is then removed in vacuo