Lithium Hydroxide → 3-[(N-Benzyloxycarbonyl-N-ethyl-amino)-methyl]-4-(5-carboxymethyl-pyridin-3-yl)-benzoic acid

HRID 554585Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 554585
C([O:8][C:9](=[O:40])[C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:17]=[N:18][CH:19]=[C:20]([CH2:22][C:23]([OH:25])=[O:24])[CH:21]=2)=[C:12]([CH2:26][N:27]([C:30]([O:32][CH2:33][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)=[O:31])[CH2:28][CH3:29])[CH:11]=1)C1C=CC=CC=1.[Li+].[OH-]>CO>[CH2:33]([O:32][C:30]([N:27]([CH2:26][C:12]1[CH:11]=[C:10]([CH:15]=[CH:14][C:13]=1[C:16]1[CH:17]=[N:18][CH:19]=[C:20]([CH2:22][C:23]([OH:25])=[O:24])[CH:21]=1)[C:9]([OH:40])=[O:8])[CH2:28][CH3:29])=[O:31])[C:34]1[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1

Komponenten

4

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

3-[(N-Benzyloxycarbonyl-N-ethyl-amino)-methyl]-4-(5-carboxymethyl-pyridin-3-yl)-benzoic acid benzyl ester (0.369 g, 0.68 mmol) was dissolved in MeOH (4 mL) and cooled to 0° C. 1N Aqueous LiOH (3 mL, 3 mmol) was added, and the reaction was stirred at room temperature for 1 hour. The mixture was quenched with 1N aqueous HCl (3 mL) and extracted with EtOAc. The combined organic layers were washed with H2O and concentrated, and the residue was purified by preparative HPLC to give Compound 1.

Aufarbeitung

  1. customThe mixture was quenched with 1N aqueous HCl (3 mL)
  2. extractionextracted with EtOAc
  3. washThe combined organic layers were washed with H2O
  4. concentrationconcentrated
  5. customthe residue was purified by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-cb6f8039faf34338b5256942566cab47
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08049015B2

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