反应详情

A suspension of 3.5 g of 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepine-2-thione, 5.5 g of glycine, 5.5 g of sodium carbonate, 100 ml of ethanol and 30 ml of water was refluxed with stirring for an hour and the mixture was poured into water. The pH of the solution was adjusted to 4 by addition of 2N hydrochloric acid and was extracted with chloroform. The mixture was filtered and the filtrate was dried over magnesium sulfate and evaporated to dryness. The gummy residue was crystallized by trituration with methanol and the mixture was filtered. The recovered solid was crystallized from ethanol to obtain 3.1 g (77% yield) of 2-carboxymethylamino-7-chloro-5-phenyl-3H-1,4-benzodiazepine melting at 215°-220° C.

1. temperaturewas refluxed
2. extractionwas extracted with chloroform
3. filtrationThe mixture was filtered
4. dry with materialthe filtrate was dried over magnesium sulfate
5. customevaporated to dryness
6. customThe gummy residue was crystallized by trituration with methanol
7. filtrationthe mixture was filtered
8. customThe recovered solid was crystallized from ethanol