1-methyl-1,4-diazepan-2-one;hydrochloride

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred mixture of (3R)-3-[(tert-butoxycarbonyl)amino]-4-(2,5-difluorophenyl)butanoic acid (40 mg), EDC (29 mg), and HOBT (21 mg) in dichloromethane was added triethylamine (0.042 mL) and hexahydro-1-methyl-2H-1,4-diazepin-2-one hydrochloride (33 mg). The resultant mixture was stirred at ambient temperature overnight and then concentrated. The residue was purified by preparative TLC (silica gel, 8% 10:1 methanol/concentrated ammonium hydroxide in dichloromethane) to yield the title compound. concentrated The residue was purified by preparative TLC (silica gel, 8% 10:1 methanol/concentrated ammonium hydroxide in dichloromethane)

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred mixture of (3R)-3-[(tert-butoxycarbonyl)amino]-4-(2,5-difluorophenyl)butanoic acid (40 mg), EDC (29 mg), and HOBT (21 mg) in dichloromethane was added triethylamine (0.042 mL) and hexahydro-1-methyl-2H-1,4-diazepin-2-one hydrochloride (33 mg). The resultant mixture was stirred at ambient temperature overnight and then concentrated. The residue was purified by preparative TLC (silica gel, 8% 10:1 methanol/concentrated ammonium hydroxide in dichloromethane) to yield the title compound. concentrated The residue was purified by preparative TLC (silica gel, 8% 10:1 methanol/concentrated ammonium hydroxide in dichloromethane)