Ammonia → HCID 86603523, compound

At room temperature, NH3 (96 mL, 670 mmol, 7N in methanol) was added subsurface via syringe to a stirred slurry of semicarbazide hydrochloride (50 g, 450 mmol) in methanol (375 mL). After one hour, the solution was filtered to remove ammonium chloride. The filtrate was diluted with ethyl acetate (750 mL) and the resulting solution was concentrated to ˜400 mL by a reduced pressure distillation. The solution was filtered and treated with methane sulfonic acid (47.4 g, 490 mmol). Upon acid addition, a white precipitate formed which was collected by filtration. The solid was rinsed with ethyl acetate (200 mL) and dried under reduced pressure.

1. filtrationthe solution was filtered
2. customto remove ammonium chloride
3. additionThe filtrate was diluted with ethyl acetate (750 mL)
4. concentrationthe resulting solution was concentrated to ˜400 mL by a reduced pressure distillation
5. filtrationThe solution was filtered
6. additionUpon acid addition
7. customa white precipitate formed which
8. filtrationwas collected by filtration
9. washThe solid was rinsed with ethyl acetate (200 mL)
10. customdried under reduced pressure

ORD record

ord-22391251c31e4366833b8dc0ad206632

Source dataset

uspto-grants-2007_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07235671B2