反应详情

A solution of 2.0 g (5.6 mmole) of 9-chloro-7-(2-chlorophenyl)-2-methyl-5H-pyrimido[5,4-d][2]benzazepine and 2.2 g (10.8 mmole) of 85% meta-chloroperbenzoic acid in 100 ml of methylene chloride was stirred at room temperature for 21 hr. The methylene chloride solution was washed with cold dilute aqueous sodium hydroxide, dried over anhydrous sodium sulfate, and concentrated at reduced pressure to dryness. Purification by plug filtration (silica gel, 25 g; eluent 1000 ml 1:1 ether methylene chloride) gave a colorless solid, mp 215°-216° C.

1. washThe methylene chloride solution was washed with cold dilute aqueous sodium hydroxide
2. dry with materialdried over anhydrous sodium sulfate
3. concentrationconcentrated at reduced pressure to dryness
4. customPurification
5. filtrationby plug filtration (silica gel, 25 g; eluent 1000 ml 1:1 ether methylene chloride)
6. customgave a colorless solid, mp 215°-216° C.