1,2-Dichloroethane → HCID 59591388, compound

Participants

Reaction Steps

To 2-fluoro-5-{[(2,2,2-trifluoroethyl)amino]sulfonyl}benzoic acid (intermediate 25)(30.1 mg 0.1 mmol) and above 5-[1-(4-fluorophenyl)-1-methylethyl]-1,3,4-thiadiazol-2-amine (23.7 mg, 0.1 mmol) in 2.0 mL of mixed solvent (DCM:DMF=10:1) were added EDC (19.2 mg, 0.1 mmol) and HOAt (13.6 mg, 0.1 mmol). The resultant mixture was stirred at room temperature for overnight, and then concentrated in vacuo. The residue was purified by using a Gilson preparative HPLC system with a Waters Xterra (C-18) column 100 mm by 50 mm ID, eluting with 20% B to 99% B in 10 min, where A=H2O and B=CH3CN pumped at 150 mL/min to yield 5-[(ethylamino)sulfonyl]-2-fluoro-N-[5-(1-methyl-1-phenylethyl)-1,3,4-thiadiazol-2-yl]benzamide (2.6 mg).

Provenance & Evidence