反应详情

A mixture of 0.5 g (1.3 mmol) of 9-chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-6-oxide and 1.0 ml (10 mmol) of phosphorous trichloride in 20 ml of methylene chloride was refluxed for 3 hr. The mixture was cooled, poured over ice, basified with ammonium hydroxide and extracted with methylene chloride. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and concentrated at reduced pressure. The residue crystallized upon the addition of ether to give colorless prisms, mp 121°-123° C.

1. temperaturewas refluxed for 3 hr
2. temperatureThe mixture was cooled
3. additionpoured over ice
4. extractionextracted with methylene chloride
5. washThe methylene chloride solution was washed with water
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated at reduced pressure
8. customThe residue crystallized upon the addition of ether
9. customto give colorless prisms, mp 121°-123° C.