HCID 178423619, compound → HCID 178423621, compound

Participants

Reaction Steps

Charge a flask with Trans-4-[[(5S)-5-[[[3,5-bis(trifluoromethyl)phenyl]methyl](2-methyl-2H-tetrazol-5-yl)amino]-2,3,4,5-tetrahydro-7,9-dimethyl-1H-1-benzazepin-1-yl]methyl]-cyclohexanecarboxylic acid (15.87 kg) and water (158.8 L). Stir the resulting mixture at RT for 2 hrs. Thereafter filter the resulting mixture to collect the solids. Dry the solids over night. The resulting solids were dissolved in MeOH heated to about 65-70° C. for 2 hrs to provide a clear solution. Filter the clear solution, then cool the filtrate to about 0 to 5° C. to induce crystallization. Collect the resulting crystals, and dry overnight. Suspend the crystalline material in water (158.8 L) and stir for about 2 hrs at RT. Collect the crystalline solid; dry at high vacuum at 40-45° C. to provide a solid that exhibits a water content of between 2.7 to 3.1 as determined by the Karl Fischer method.

Provenance & Evidence