Hydrochloric Acid → HCID 69196674, compound

To the solution of tert-butyl 1-cyclopropyl-3-(cyclopropylamino)-3-oxopropylcarbamate (38.10 g, 150 mmol) in dichloromethane (600 mL) and methyl alcohol (40 mL) was added 2 M solution of hydrochloric acid in diethyl ether (300 mL, 600 mmol) with an addition funnel at such a rate that the temperature of the reaction remained below 30° C. The reaction was allowed to stir at room temperature overnight. After 18 h, the reaction was complete as indicated by ELSD/MS. The reaction mixture was evaporated under reduced pressure. Diethyl ether (2×200 mL) was added to the residue, and the mixture was stirred for 15 min, and then decanted. This process was repeated to remove excess of hydrochloric acid. It was further dried in a vacuum oven overnight to afford 3-amino-N,3-dicyclopropylpropanamide hydrochloride (30 g, >100% yield).

1. customremained below 30° C
2. waitAfter 18 h
3. customThe reaction mixture was evaporated under reduced pressure
4. additionDiethyl ether (2×200 mL) was added to the residue
5. stirringthe mixture was stirred for 15 min
6. customdecanted
7. customto remove excess of hydrochloric acid
8. customIt was further dried in a vacuum oven overnight

ORD record

ord-55caa16b36ff44289fba0e2170935be5

Source dataset

uspto-grants-2008_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07468375B2