Hydrochloric Acid → 3-(S)-Amino-1-(1-chloro-isoquinolin-7-ylmethyl)-pyrrolidin-2-one hydrochloride

HRID 651593

Reaktionsgleichung

Reaktionsgleichung von HRID 651593
C(OC(=O)[NH:7][C@H:8]1[CH2:12][CH2:11][N:10]([CH2:13][C:14]2[CH:23]=[C:22]3[C:17]([CH:18]=[CH:19][N:20]=[C:21]3[Cl:24])=[CH:16][CH:15]=2)[C:9]1=[O:25])(C)(C)C.Cl>CCOC(C)=O>[ClH:24].[NH2:7][C@H:8]1[CH2:12][CH2:11][N:10]([CH2:13][C:14]2[CH:23]=[C:22]3[C:17]([CH:18]=[CH:19][N:20]=[C:21]3[Cl:24])=[CH:16][CH:15]=2)[C:9]1=[O:25]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 54049378[1-(1-Chloro-isoquinolin-7-ylmethyl)-2-oxopyrrolidin-3(S)-yl]-carbamic acid tert-butyl ester

Produkt 1

HCID 206807083-(S)-Amino-1-(1-chloro-isoquinolin-7-ylmethyl)-pyrrolidin-2-one hydrochlorideAusbeute 200 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of [1-(1-chloro-isoquinolin-7-ylmethyl)-2-oxopyrrolidin-3(S)-yl]-carbamic acid tert-butyl ester (2.1 g, 5.6 mmol) in EtOAc (170 mL) at 0° C. is bubbled HCl gas for 5 minutes. The solution is stirred at 0° C. for 15 minutes, then the ice bath is removed and the solution allowed to warn to room temperature. After 4 hours at room temperature, the solution is concentrated and the remaining solid is washed with ether to give the title compound (1.74 g, 5.6 mmol) as a pale yellow solid.

Aufarbeitung

  1. customthe ice bath is removed
  2. customto warn to room temperature
  3. waitAfter 4 hours at room temperature
  4. concentrationthe solution is concentrated
  5. washthe remaining solid is washed with ether

Quellen und Nachweise

ORD-Eintrag
ord-d0b56a0b486644ca9bd4439b8b3becfc
Quelldatensatz
uspto-grants-2001_08
Patentnummer
US06281227B1

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