反应详情

温度

150 °C

Thiourea (7.56 g) and iodine (12.61 g) are mixed and stirred mechanically under a stream of nitrogen. To this mixture is added 4-[2-[4-(2-pyridinyl)-1-piperazinyl]ethyl]cyclohexanone (9.52 g) (Example J) and the temperature gradually increased to 150° C. Following 30 minutes at this temperature, the mixture is cooled to room temperature and treated with 250 ml of a 10% solution of hydrochloric acid. Some insoluble material is filtered, the filtrate made basic with ammonium hydroxide, and extracted with chloroform (2×500 ml). The combined organic extracts are dried over magnesium sulfate and concentrated. The crude reaction mixture is purified by MPLC (silica; 5% methanol, 95% chloroform) to give the title compound as a light yellow solid; mp 194°-197° C.

1. temperaturethe mixture is cooled to room temperature
2. filtrationSome insoluble material is filtered
3. extractionextracted with chloroform (2×500 ml)
4. dry with materialThe combined organic extracts are dried over magnesium sulfate
5. concentrationconcentrated
6. customThe crude reaction mixture
7. customis purified by MPLC (silica; 5% methanol, 95% chloroform)