Hydrochloric Acid → HCID 22877423, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 256 mg (0.624 mmol) of 2-benzyloxycarbonylamino-2-methyl- N-[7-amino-2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-3(R)-yl]propanamide (Step C) in 1.2 mL of water was added 0.171 mL of concentrated hydrochloric acid. The resulting mixture was stirred until all the solids were dissolved then the solution was cooled to 0° C. To this solution was added a solution of 52 mg (0.75 mmol) of sodium nitrite in a minimal amount of water. After 30 minutes at 0° C., 0.156 mL (1.06 mmol) of 60 weight percent aqueous hexafluorophosphoric acid was added dropwise. Immediately a white precipitate formed. The solids were filtered and washed with ice cold water, then air dried. The resulting solid was dried under vacuum overnight.

Provenance & Evidence