反应详情

In one portion 1.0 g (2.8 mmol) of 1,9-dichloro-3-methyl-7-phenyl-5H-pyrimido[4,5-d][2]benzazepine was added to a solution of 150 mg (3.1 mmol) of 50% mineral oil dispersion of sodium hydride and an excess of methyl mercaptan (>3.1 mmol) in 25 mL of dimethylformamide. The mixture was stirred at room temperature for 30 min and diluted with water. The resulting precipitate was collected by filtration to give a yellow solid. Recrystallization from a mixture of ether and methylene chloride gave pale yellow prisms, mp 181°-183°.

1. filtrationThe resulting precipitate was collected by filtration
2. customto give a yellow solid
3. customRecrystallization
4. additionfrom a mixture of ether and methylene chloride
5. customgave pale yellow prisms, mp 181°-183°