Water → 9-Chloro-7-[2-(2,4-di-t-amylphenoxy)butanoylamino]-6-hydroxy-1,5-benzodiazepin-2,4-dione

Participants

Reaction Steps

In 250 ml of benzene was dissolved 17 g of the resulting 2,3-diamino-4-chloro-6-[2-(2,4-di-t-amylphenoxy)butanoylamino]phenol, and a solution of 5.8 g of malonyl dichloride in 100 ml of benzene was slowly added to the solution at room temperature while stirring. After the dropwise addition, the reaction mixture was stirred for 1 hour. Water and ethyl acetate were added to the reaction mixture to effect extraction. The extract was concentrated, and the residue was purified by silica gel column chromatography (chloroform/ethyl acetate=2/1 by volume) to obtain 4.2 g of the desired coupler (Coupler 3) having a melting point of 193° to 195° C.

Provenance & Evidence