Hydrochloric Acid → trans-3-Amino-4-methoxypyrrolidine dihydrochloride

HRID 358900Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 358900
[ClH:1].[NH2:2][CH:3]1[CH:7]([O:8][CH3:9])[CH2:6][N:5](C(OC(C)(C)C)=O)[CH2:4]1>C(O)C>[ClH:1].[ClH:1].[NH2:2][C@H:3]1[C@H:7]([O:8][CH3:9])[CH2:6][NH:5][CH2:4]1

Komponenten

4

Versuchsvorschrift

6.3 ml of 6N aqueous hydrochloric acid were added to a solution of 0.4 g (0.0019 mole) of 3-amino-1-t-butoxycarbonyl-4-methoxypyrrolidine [prepared as described in Step (3) above] dissolved in 20 ml of ethanol, and the mixture was heated under reflux for 1.5 hours, after which the solvent was removed by evaporation under reduced pressure. The residue was washed with a 1:9 by volume mixture of ethanol and ethyl acetate to give 0.34 g of trans-3-amino-4-methoxypyrrolidine dihydrochloride as a colorless powder, melting at 248°~258° C. (with decomposition).

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. customafter which the solvent was removed by evaporation under reduced pressure
  4. washThe residue was washed with a 1:9 by volume mixture of ethanol and ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-995b5ec61da5453f84f27d08bd551762
Quelldatensatz
uspto-grants-1991_03
Patentnummer
US04997943

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