Sulfuric Acid → HCID 25256627, compound

Participants

Reaction Conditions

Reaction Steps

250 mg ethyl 4-[4-[(2R)-3-[4-amino-3-chloro-5-(trifluoromethyl)phenyl]-1-oxo-2-[[[4-(1,2,4,5-tetrahydro-2-oxo-3H-1,3-benzodiazepin-3-yl)-1-piperidinyl]carbonyl]oxy]propyl]-1-piperazinyl]-piperidine-1-acetate (0.316 mmol) are dissolved in 2.5 ml of ethanol at ambient temperature. The solution is heated to 80° C. and combined with 46.8 μl aqueous sulphuric acid (48%), whereupon a granular precipitate is immediately formed. The temperature is lowered by 5° C. every 30 minutes. The suspension formed is stirred for 12 hours at ambient temperature. The solid formed is filtered off, washed with ethanol and dried for 12 hours at 40° C.

Provenance & Evidence