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Ethanol → 3-[(N-benzyloxycarbonyl-N-ethyl-amino)-methyl]-4-(5-ethoxycarbonylmethyl-pyridin-3-yl)-benzoic acid ethyl ester

HRID 554586
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 554586
[CH2:1]([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)[C:2]1C=CC=CC=1.S(=O)(=O)(O)O.[CH3:46][CH2:47]O>>[CH2:1]([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]([O:25][CH2:46][CH3:47])=[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)[CH3:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 585650203-[(N-benzyloxycarbonyl-N-ethyl-amino)-methyl]-4-(5-carboxymethyl-pyridin-3-yl)-benzoic acid benzyl ester

Produkt 1

HCID 585652203-[(N-benzyloxycarbonyl-N-ethyl-amino)-methyl]-4-(5-ethoxycarbonylmethyl-pyridin-3-yl)-benzoic acid ethyl ester

Reaktionsbedingungen

Temperatur
95 °C

Versuchsvorschrift

3-[(N-Benzyloxycarbonyl-N-ethyl-amino)-methyl]-4-(5-carboxymethyl-pyridin-3-yl)-benzoic acid benzyl ester (1.74 g, 3.2 mmol) in EtOH (200 mL) was treated with sulfuric acid (2 mL), and the reaction was stirred at 95° C. for 2 hours. The mixture was cooled to room temperature and concentrated, and the residue was partitioned between EtOAc and H2O. The solution was extracted with EtOAc, and the combined organic layers were washed with 1N aqueous HCl and concentrated. The crude material was purified by silica gel chromatography (0-100% EtOAc in hexanes) to give 3-[(N-benzyloxycarbonyl-N-ethyl-amino)-methyl]-4-(5-ethoxycarbonylmethyl-pyridin-3-yl)-benzoic acid ethyl ester.

Aufarbeitung

  1. temperatureThe mixture was cooled to room temperature
  2. concentrationconcentrated
  3. customthe residue was partitioned between EtOAc and H2O
  4. extractionThe solution was extracted with EtOAc
  5. washthe combined organic layers were washed with 1N aqueous HCl
  6. concentrationconcentrated
  7. customThe crude material was purified by silica gel chromatography (0-100% EtOAc in hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-d6bb91ec556e4bd586f60a4c496477bb
Quelldatensatz
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08049015B2

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