HRID1904226

反应详情

EQUATION

反应方程式

HRID 1904226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.3 g (0.1 mol) of (2-oxo-1-pyrrolidinyl)acetic acid and 16.2 g (0.1 mol) of N,N'-carbonyldiimidazole are heated under reflux in 70 ml of tetrahydrofuran for 15 min. After cooling, 13.8 g (0.1 mol) of 1-(2-aminoethyl)-2,5-dimethylpyrrole in 70 ml of tetrahydrofuran are added dropwise. After the reactionmixture has been stirred at room temperature for 6 h, it is concentrated, acifified with dilute acetic acid and extracted with methylene chloride. The methylene chloride extract is concentrated, and the residue is triturated with ether, filtered off with suction and recrystallized from dibuyl ether. Yield: 9.0 g (34% of theory), Melting point: 109°-111° C. Elemental analysis: C14H21N3O2 (263.34) calculated: C 63.9 H 8.0 N 16.0 O 12.2 found: C 63.8 H 8.0 N 15.9 O 12.2

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationit is concentrated
  3. extractionextracted with methylene chloride
  4. extractionThe methylene chloride extract
  5. concentrationis concentrated
  6. customthe residue is triturated with ether
  7. filtrationfiltered off with suction
  8. customrecrystallized from dibuyl ether