Salicylic Acid → HCID 25256628, 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 1.5 ml of ethanol at ambient temperature. The solution is heated to 80° C. and combined with a solution of 43 mg salicylic acid (0.361 mmol) in 1.5 ml of ethanol. The temperature is lowered by 5° C. every 30 minutes. Then the solution is stirred for 12 hours at ambient temperature. As no precipitate has formed, the solvent is distilled off and the residue is dissolved in 2.5 ml methylisobutylketone at 80° C. The temperature is lowered by 5° C. every 30 minutes. Then the solution is stirred for 12 hours at ambient temperature. Then the solution is stirred for a further 24 hours in the open vessel during which time the solvent evaporates. The resultant solid is filtered off, washed with methylisobutylketone and dried for 12 hours at 35° C.

Provenance & Evidence