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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 69411675, Verbindung

HRID 889846
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 889846
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][NH:11][C:12](=[O:22])[C:13]3[CH:14]=[C:15]([CH:19]=[CH:20][CH:21]=3)[C:16]([OH:18])=O)=[CH:9][C:4]=2[O:3][CH2:2]1.O.ON1[C:29]2C=CC=C[C:28]=2N=N1.C([N:36]([CH2:41][C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1)[CH2:37][C:38]([OH:40])=[O:39])C.Cl.CN(C)CCCN=C=NCC>C(Cl)Cl.O>[CH2:28]([O:40][C:38](=[O:39])[CH2:37][N:36]([C:16](=[O:18])[C:15]1[CH:19]=[CH:20][CH:21]=[C:13]([C:12](=[O:22])[NH:11][CH2:10][C:8]2[CH:7]=[CH:6][C:5]3[O:1][CH2:2][O:3][C:4]=3[CH:9]=2)[CH:14]=1)[CH2:41][C:42]1[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=1)[CH3:29]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 19755290Glycine, N-ethyl-N-(phenylmethyl)-HCID 22248625HCID 22248625, Verbindung

Produkt 1

HCID 69411675HCID 69411675, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 6344DichloromethaneLösungsmittel

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. customthe organic phase separated
  2. washwashed with 10% citric acid (100 mL), saturated sodium bicarbonate (100 mL) and brine (100 mL)
  3. dry with materialThe organic phase dried over magnesium sulfate
  4. customevaporated at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-0bbc5fbc187949c99386d45c97da8f96
Quelldatensatz
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06995151B2

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