反应详情

A mixture of 1.1 g (3.0 mmole) of 9-chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepin-2-thiol, 1.0 ml (10 mmole) of dimethyl sulfate, 20 ml of 1N sodium hydroxide and 10 ml of ethanol was stirred at room temperature for 15 min. The mixture was diluted with water and extracted with methylene chloride. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to give an oil. Crystallization from ether gave colorless prisms, mp 187°-188° C.

1. extractionextracted with methylene chloride
2. dry with materialThe methylene chloride solution was dried over anhydrous sodium sulfate
3. concentrationconcentrated at reduced pressure
4. customto give an oil
5. customCrystallization from ether
6. customgave colorless prisms, mp 187°-188° C.