Ethylenediamine → N-(2-Aminoethyl)-1,3-benzodioxole-5-carboxamide

HRID 2255110

Reaktionsgleichung

Reaktionsgleichung von HRID 2255110
[CH2:1]1[O:13][C:12]2[CH:11]=[CH:10][C:5]([C:6]([O:8]C)=O)=[CH:4][C:3]=2[O:2]1.[CH2:14]([NH2:17])[CH2:15][NH2:16]>>[NH2:16][CH2:15][CH2:14][NH:17][C:6]([C:5]1[CH:10]=[CH:11][C:12]2[O:13][CH2:1][O:2][C:3]=2[CH:4]=1)=[O:8]

Komponenten

3

Edukt 2

HCID 3301EthylenediamineHCID 67590Methyl piperonylate

Produkt 1

HCID 13536947N-(2-Aminoethyl)-1,3-benzodioxole-5-carboxamideAusbeute 41,9 %

Versuchsvorschrift

7 g (0.039 mol) of methyl 3,4-methylenedioxybenzoate and 8.5 ml (0.126 mol) of ethylenediamine are heated to 100° (bath temperature) for 2.5 hours. After cooling, the excess ethylenediamine is removed in a high vacuum. The residue is acidified with dilute hydrochloric acid and extracted with chloroform. The aqueous phase is made alkaline with sodium hydroxide solution and then extracted several times with chloroform. After evaporating the solvent and recrystallizing the residue from chloroform/hexane, there are obtained 3.4 g of N-(2-aminoethyl)-1,3-benzdioxol-5-carboxamide, m.p. 120°-123°. The hydrochloride melts at 210°-213°.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe excess ethylenediamine is removed in a high vacuum
  3. extractionextracted with chloroform
  4. extractionextracted several times with chloroform
  5. customAfter evaporating the solvent
  6. customrecrystallizing the residue from chloroform/hexane, there

Quellen und Nachweise

ORD-Eintrag
ord-538bdc0098a6475585cbe34c26b942c0
Quelldatensatz
uspto-grants-1993_08
Patentnummer
US05238962

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