Sulfuric Acid → HCID 69058084, compound

Participants

Reaction Steps

0.5 g (0.69 mmol) (R)-1-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-2-[4-(4-methyl-piperazin-1-yl)-piperidin-1-yl]-2-oxo-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate are dissolved in 10 ml of methanol at ambient temperature. After the addition of 100 μl sulphuric acid (48% in water) the mixture is stirred for 3 hours at ambient temperature. After about 5 ml of methanol has been evaporated off, 1 ml of tert-butylmethylether is added, whereupon an oil is precipitated. After removal of the supernatant solvent the residue is combined with 5 ml acetone, during which time crystallisation sets in. The precipitate formed is filtered and dried for 12 hours at 30° C.

Provenance & Evidence