Aluminum(III) Chloride → HCID 136016305, compound

Participants

Reaction Steps

A solution of 1.00 g (0.0263 mole) of 7-bromo-5-(2-chlorophenyl)-1,3-dihydro-8-methoxy-2H-1,4-benzodiazepin-2-one (Id) in 85 mL of 1,2-dichloroethane was stirred overnight with 1.053 g (0.0079 mole) of aluminum trichloride. An additional 1.00 g of aluminum trichloride was added, and the mixture stirred overnight, after which time the mixture was poured into ice water. The mixture was extracted with dichloromethane-methanol, and the organic layer washed twice with water and then dried over anhydrous sodium sulfate. The solution was concentrated under reduced pressure to provide 0.700 g of 7-bromo-5-(2-chlorophenyl)-1,3-dihydro-8-hydroxy-2H-1,4-benzodiazepin-2-one (Ipp) (MH+/Z=465), which was of sufficient purity to be used in the next step.

Provenance & Evidence