Hydrochloric Acid → HCID 59200469, compound

Participants

Reaction Steps

A solution of methyl 3-fluoro-4-(2-(thieno[3,2-c]pyridin-4-ylamino)thiazol-5-ylthio)picolinate (3.13 g, 7.48 mmol) was treated with aqueous sodium hydroxide (1N, 12 mL, 12.0 mmol) and was stirred at room temperature for 2 hours. The reaction was then acidified to pH ˜6 with 10% aqueous HCl and then poured into water (300 mL) and allowed to sit overnight for complete precipitation. The solid was collected by filtration, washed with water and air dried to give the title material (1.86 g, 62%). 1H NMR (400 MHz, DMSO-d6) δ ppm: 12.24 (1H, s), 8.22 (1H, d, J=5.56 Hz), 8.18 (1H, d, J=5.05 Hz), 8.15 (1H, d, J=5.81 Hz), 7.90 (1H, s), 7.87 (1H, d, J=5.56 Hz), 7.69 (1H, d, J=5.56 Hz), 6.94 (1H, t, J=5.31 Hz). LC/MS (M+H)+: 405. HPLC ret. time (Condition I): 1.28 min.

Provenance & Evidence