Acetic Acid → HCID 17747530, compound

Participants

Reaction Steps

50 mg (0.077 mmol) 2-(4-piperazin-1-yl-phenylamino)-4-((S)-4-oxo-2,3,10,10a-tetrahydro-1H.4H-9-oxa-3a-aza-benzo[f]azulen-5-ylamino)-5-trifluoromethyl-pyrimidine are dissolved in 0.5 mL dimethylformamide and combined with 12 μL (0.154 mmol) formaldehyde and 2 μL (0.039 mmol) acetic acid. 86 mg (0.385 mmol) of sodium triacetoxyborohydride are metered into this mixture and it is stirred for 16 h at ambient temperature. Then the solvent is eliminated in vacuo. The crude product is purified by column chromatography. The carrier material used is C18-RP-silica gel and a gradient is run through which at the starting point consists of 95% water and 5% acetonitrile and at the end point consists of 5% water and 95% acetonitrile. 0.2% Formic acid is added to the two eluants. The suitable fractions are combined with 1 N aqueous hydrochloric acid and freeze-dried.

Provenance & Evidence