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1,4-Dioxane hydrochloride → [(4-Aminomethyl-benzyl)-(4-dipropylamino-butyl)-amino]-acetic acid ethyl ester

HRID 2080858
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2080858
[CH2:1]([O:3][C:4](=[O:34])[CH2:5][N:6]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([CH2:25][NH:26]C(OC(C)(C)C)=O)=[CH:21][CH:20]=1)[CH2:7][CH2:8][CH2:9][CH2:10][N:11]([CH2:15][CH2:16][CH3:17])[CH2:12][CH2:13][CH3:14])[CH3:2].Cl.O1CCOCC1>C(O)C>[CH2:1]([O:3][C:4](=[O:34])[CH2:5][N:6]([CH2:18][C:19]1[CH:20]=[CH:21][C:22]([CH2:25][NH2:26])=[CH:23][CH:24]=1)[CH2:7][CH2:8][CH2:9][CH2:10][N:11]([CH2:12][CH2:13][CH3:14])[CH2:15][CH2:16][CH3:17])[CH3:2]
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Komponenten

4

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 67103729[[4-(t-Butoxycarbonylamino-methyl)-benzyl]-(4-dipropylamino-butyl)-amino]-acetic acid ethyl ester

Produkt 1

HCID 59850563[(4-Aminomethyl-benzyl)-(4-dipropylamino-butyl)-amino]-acetic acid ethyl esterAusbeute 97,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

The compound (21.265 g) obtained in Example 72-1 was dissolved in ethanol (100 ml) and added with a 4 mol/l hydrogen chloride/dioxane solution (140 ml) and the whole was stirred at room temperature for 1 hour. Subsequently, the solution was stirred at 40° C. for 1 hour. After completion of the reaction, the solvent was distilled off. The resultant was added with a 1 mol/l sodium hydroxide aqueous solution to make the pH thereof to 12. The solution was subjected to extraction with chloroform and dried with magnesium sulfate. The solvent was distilled off, thereby obtaining the subject compound (16.46 g) as a colorless oily substance.

Aufarbeitung

  1. stirringSubsequently, the solution was stirred at 40° C. for 1 hour
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off
  4. additionThe resultant was added with a 1 mol/l sodium hydroxide aqueous solution
  5. extractionThe solution was subjected to extraction with chloroform
  6. dry with materialdried with magnesium sulfate
  7. distillationThe solvent was distilled off

Quellen und Nachweise

ORD-Eintrag
ord-47c3fc6e4ed844338ed95155a7573b82
Quelldatensatz
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07932281B2

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