HRID35069

反应详情

EQUATION

反应方程式

HRID 35069 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-[3-(1-piperidinylmethyl)phenoxy]butanal (522 mg) and 3,5-diamino-1,2,4-triazole (200 mg) in absolute ethanol (20 ml) was heated under reflux for 2 h. The cooled solution was treated with sodium borohydride (200 mg) and stirred at room temperature for 18 hr. The mixture was evaporated in vacuo and the residue partitioned between ethyl acetate and water. The combined organic extracts were evaporated in vacuo and the residue was chromatographed on silica with methanol as eluant to give the title compound as an oil (250 mg), TLC silica (ethyl acetate:isopropanol:water:ammonia 25:15:8:2) 0.4, NMR (CDCl3) 2.8 t (1H); 3.0-3.3 m (3H); 5.3 m (2H); 6.2 m (2H); 6.6-6.8 m (4H); 7.7 m (4H); 8.0-8.8 m (10H).

WORKUP

后处理

  1. temperatureunder reflux for 2 h
  2. customThe mixture was evaporated in vacuo
  3. customthe residue partitioned between ethyl acetate and water
  4. customThe combined organic extracts were evaporated in vacuo
  5. customthe residue was chromatographed on silica with methanol as eluant