反应详情

A stirred suspension of 3 g (0.0075 mole) of 8-chloro-6-(2-chlorophenyl)-1,2-dihydro-2-methyl-1-oxo-4H-imidazo[1,5-a][1,4]benzodiazepin-3-carboxylic acid in 90 ml of methylene chloride was cooled in an ice bath and treated with 1.9 g (0.009 mole) of phosphorus pentachloride in portions. Stirring in the cold under a drying tube was continued for 30 min. Ammonia was then bubbled into the cold solution for 5 min and stirring in the cold was continued 30 min. longer. Evaporation at reduced pressure gave a tan solid. The solid was stirred with 3N ammonium hydroxide and extracted with methylene chloride. An emulsion formed but was destroyed by filtering to remove some high melting solid. The methylene chloride layer was dried over sodium sulfate and evaporated to give a yellow solid which was recrystallized from benzene to give off-white needles with mp 158°-160°. Uv λ sh 215 mμ (ε=43000) max 272 (15500) sh 330 (2500); ir (CHCl3); ir (CHCl3) 3510, 3400 cm-1 (NH2) 1703 (CO) 1685 (CONH2).

1. temperaturewas cooled in an ice bath
2. customAmmonia was then bubbled into the cold solution for 5 min
3. stirringstirring in the cold
4. waitwas continued 30 min.
5. customEvaporation at reduced pressure
6. customgave a tan solid
7. extractionextracted with methylene chloride
8. customAn emulsion formed
9. customwas destroyed
10. filtrationby filtering
11. customto remove some high melting solid
12. dry with materialThe methylene chloride layer was dried over sodium sulfate
13. customevaporated
14. customto give a yellow solid which
15. customwas recrystallized from benzene
16. customto give off-white needles with mp 158°-160°