HRID2071656

反应详情

EQUATION

反应方程式

HRID 2071656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To stirred liquid ammonia (300 mls) was added ferric nitrate (50 mgs) followed by sodium metal (4.5 gms). The mixture was allowed to stand for 30 minutes and then 3-(4-pyridyl)-1-amino propane (13.5 gms) was added. A deep yellow colour was allowed to develop over 1 hour and ethylene oxide (5.0 gms) was then added. The mixture was stirred for a further 2 hours after which time solid ammonium chloride (12 gms) was added. The solvent was allowed to evaporate overnight and the residual solid was extracted into pyridine. Evaporation of the pyridine and crystallisation of the residue from benzene yielded 3-(4-pyridyl)-1-amino-5-hydroxy pentane (3.4 gms; 17%). Characterised by the following spectral data:

WORKUP

后处理

  1. waitto develop over 1 hour
  2. additionwas added
  3. customto evaporate overnight
  4. extractionthe residual solid was extracted into pyridine
  5. customEvaporation of the pyridine and crystallisation of the residue from benzene