Hydrochloric Acid → HCID 20607351, Verbindung

HRID 431027Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 431027
[ClH:1].C(OC([NH:9][C@H:10]1[C@@H:14]([CH2:15][F:16])[CH2:13][NH:12][CH2:11]1)=O)(C)(C)C>O>[ClH:1].[ClH:1].[NH2:9][C@H:10]1[C@@H:14]([CH2:15][F:16])[CH2:13][NH:12][CH2:11]1

Komponenten

4

Versuchsvorschrift

Concentrated hydrochloric acid (1 ml) was added to 3-(S)-tert-butoxycarbonylamino-4-(S)-fluoromethylpyrrolidine (441 mg, 2.02 mmol) which was cooled in an ice bath, and the mixture was stirred for 10 minutes. The reaction solution was mixed with water (5 ml) and washed with dichloromethane (5 ml×3) and diethyl ether (5 ml×1). The aqueous layer was concentrated under a reduced pressure, and the resulting residue was purified by its recrystallization from methanol to give 288 mg (75%) of the title compound in the form of white crystals.

Aufarbeitung

  1. temperaturewas cooled in an ice bath
  2. washwashed with dichloromethane (5 ml×3) and diethyl ether (5 ml×1)
  3. concentrationThe aqueous layer was concentrated under a reduced pressure
  4. customthe resulting residue was purified by its recrystallization from methanol

Quellen und Nachweise

ORD-Eintrag
ord-94292d966f7749279370642b78e9310f
Quelldatensatz
uspto-grants-2003_12
Patentnummer
US06656952B2

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