HRID2255110

反应详情

EQUATION

反应方程式

HRID 2255110 的结构方程式

PROCEDURE

实验过程

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°.

WORKUP

后处理

  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