HRID248906

反应详情

EQUATION

反应方程式

HRID 248906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-amino-1-[(6-fluoro-2-naphthalenyl)methyl]piperidine (1.3 g, 5 mmol), 4-pyridoylurea (0.9 g, 5 mmol) and pyridine (6 ml) was stirred at reflux for 16 hours. The solution was diluted with water (8 ml) and the precipitated dark brown product collected by filtration to give 1.5 g. The crude product was dissolved in chloroform (25 ml), shaken with decolourising charcoal, filtered and evaporated. The residue was suspended in hot ethanol (20 ml) and succinic acid (0.44 g) added to give a clear solution which crystallised on standing. The product crystals were collected by filtration and washed with ethanol to give the succinate salt of the title compound. m.p. 187°-188° C.

WORKUP

后处理

  1. temperatureat reflux for 16 hours
  2. filtrationthe precipitated dark brown product collected by filtration
  3. customto give 1.5 g
  4. filtrationfiltered
  5. customevaporated
  6. additionsuccinic acid (0.44 g) added
  7. customto give a clear solution which
  8. customcrystallised
  9. filtrationThe product crystals were collected by filtration
  10. washwashed with ethanol