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

HRID 2255110ノート

反応式

HRID 2255110 の反応式
[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]

参加物

3

反応物 2

HCID 3301EthylenediamineHCID 67590Methyl piperonylate

生成物 1

HCID 13536947N-(2-Aminoethyl)-1,3-benzodioxole-5-carboxamide収率 41.9%

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-538bdc0098a6475585cbe34c26b942c0
出典データセット
uspto-grants-1993_08
特許番号
US05238962

反応ノート

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