Hydrochloric Acid → HCID 67497038, compound

Participants

Reaction Steps

To a 200 ml flask was added 640 mg of (S)-2-(1-(1-methyl-3-(pyridin-4-yl)-1H-pyrazol-5-ylamino)-1-oxo-3-phenylpropan-2-ylamino)acetic acid diTFA, 20 ml of dioxane, 20 drops of water and then slowly 3 ml of hydrogen chloride (2.0 M in diethyl ether). The solvent was then removed using a rotary evaporator and placed under high vacuum to give 565 mg (S)-2-(1-(1-methyl-3-(pyridin-4-yl)-1H-pyrazol-5-ylamino)-1-oxo-3-phenylpropan-2-ylamino)acetic acid dihydrochloride as an off white solid. The product was redissolved in 10% MeOH in DCM and the solvent was then removed using a rotary evaporator and placed under high vacuum to give 505 mg of 17.8 as a white solid. MS ESI (pos.) m/e: 380.2 (M+H); 1H NMR (400 MHz, CD3OD) δ ppm 8.52 (d, J=6.50 Hz, 2H), 7.72-7.89 (m, 2H), 7.25-7.47 (m, 5H), 6.65-6.81 (m, 1H), 4.17 (dd, J=8.80, 6.46 Hz, 1H), 3.51-3.57 (m, 4H), 3.41-3.51 (m, 1H), 3.28 (d, J=6.26 Hz, 1H), 3.10-3.23 (m, 1H).

Provenance & Evidence