反应详情

温度

90 °C

More specifically, 0.24 mg (1.5 mmol) of 2-fluorooctanoic acid was added to 2 ml of thionyl chloride and the mixture was refluxed at 90° C. for 2 hours. Then, the excess of thionyl chloride was distilled off, and a preliminarily prepared solution of 0.34 g (3.0 mmol) of triethylenediamine and 0.47 g (1.5 mmol) of 5-n-decyl-2-(p-hydroxyphenyl)pyrimidine in 5 ml of dry benzene was quickly added thereto, followed by 2 hours of stirring at 50° C. Thereafter, 0.06 g (1.5 mmol) of sodium hydride (60%) was added, and the mixture was further refluxed for 2 hours at 90° C. After the reaction, 2N-hydrochloric acid was added to the system, which was then subjected to extraction with benzene. The extract was dried, subjected to distillation of the solvent and purified by column chromatography with benzene to obtain 0.44 g (0.96 mmol) of 5-n-decyl-2-[4-(2-fluorooctanoyloxy)phenyl]pyrimidine. Yield: 64%

1. distillationThen, the excess of thionyl chloride was distilled off
2. temperaturethe mixture was further refluxed for 2 hours at 90° C
3. additionwas added to the system, which
4. extractionwas then subjected to extraction with benzene
5. customThe extract was dried
6. distillationsubjected to distillation of the solvent
7. custompurified by column chromatography with benzene