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Water → HCID 69410937, Verbindung

HRID 889847
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 889847
C([O:3][C:4](=[O:35])[CH2:5][N:6]([C:14](=[O:34])[C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([C:21](=[O:33])[NH:22][CH2:23][C:24]2[CH:32]=[CH:31][C:27]3[O:28][CH2:29][O:30][C:26]=3[CH:25]=2)[CH:16]=1)[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)C.O.O1CCOCC1.[OH-].[Na+]>C(O)C>[O:28]1[C:27]2[CH:31]=[CH:32][C:24]([CH2:23][NH:22][C:21]([C:17]3[CH:16]=[C:15]([CH:20]=[CH:19][CH:18]=3)[C:14]([N:6]([CH2:5][C:4]([OH:35])=[O:3])[CH2:7][C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)=[O:34])=[O:33])=[CH:25][C:26]=2[O:30][CH2:29]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 312751,4-DioxaneHCID 69411675HCID 69411675, Verbindung

Produkt 1

HCID 69410937HCID 69410937, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of N-benzo[1,3]dioxol-5-ylmethyl-isophthalamic acid (3.0 g, 10 mmol) in methylene chloride was added 1-hydroxy-benzotriazole monohydrate (“HOBt”) (1.35 g, 10 mmol) and ethyl N-benzylglycine (1.94 g, 10 mmol). To this was added 1-(3-dimethylamino-propyl)-3-ethylcarbodiimide hydrochloride (“EDAC”) (1.92 g, 10 mmol) and the mix stirred at room temperature for 24 hours. The solution treated with water (150 mL) and the organic phase separated, washed with 10% citric acid (100 mL), saturated sodium bicarbonate (100 mL) and brine (100 mL). The organic phase dried over magnesium sulfate and evaporated at reduced pressure to give ({3-[(1,3-benzodioxol-5-ylmethyl)-carbamoyl]-benzoyl}-benzyl-amino)-acetic acid ethyl ester as a solid, 3.69 g. To a solution of this ester (3.6 g, 7.6 mmol) in a mix of water (15 mL), dioxane (60 mL) and ethanol (20 mL) was added sodium hydroxide (0.72 g, 18 mmol). The mixture stirred at 50° C. for 24 hours. The solution cooled to room temperature and evaporated at reduced pressure free of solvents. The residue was diluted with water (100 mL) and washed with ether (2×50 mL). The ether discarded and the aqueous phase made acidic with 6N HCl. This was extracted with ethyl acetate (2×100 mL). The organic phases washed with brine (100 mL) and dried over magnesium sulfate. The solvent was evaporated at reduced pressure to give the title compound, 3.41 g. Microanalysis (C25H22N2O6.0.3 H2O): Calc'd: C=66.45, H=5.05, N=6.20. Found: C=66.25, H=5.15, N=5.99.

Aufarbeitung

  1. temperatureThe solution cooled to room temperature
  2. customevaporated at reduced pressure free of solvents
  3. additionThe residue was diluted with water (100 mL)
  4. washwashed with ether (2×50 mL)
  5. extractionThis was extracted with ethyl acetate (2×100 mL)
  6. washThe organic phases washed with brine (100 mL)
  7. dry with materialdried over magnesium sulfate
  8. customThe solvent was evaporated at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d1c267188fdd472c9f190ff540b2a1d5
Quelldatensatz
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06995151B2

Notizen zur Reaktion

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