HRID49802

反应详情

EQUATION

反应方程式

HRID 49802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Isobutylamine (5.1 ml, 51.2 mmol) was added to a solution of 4-(2,3-epoxypropoxy) nitrobenzene (obtained as described in Synthetic Communications, 1994, 24, 833; 1.0 g, 5.12 mmol) in THF (1 ml). The solution was heated under reflux for 3 hours and then volatile material was removed by evaporation. The residue was dissolved in methanol (5 ml) and 10% palladium on carbon (0.50 g) and ammonium formate (3.23 g, 51.2 mmol) were added. The mixture was heated under reflux for 3 hours and then filtered through diatomaceous earth. The filtrate was concentrated under reduced pressure to give the product as dark brown oil (1.22 g, 100%), which was used without further purification. MS (MH+): 238.9.

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureunder reflux for 3 hours
  3. customvolatile material was removed by evaporation
  4. dissolutionThe residue was dissolved in methanol (5 ml)
  5. temperatureThe mixture was heated
  6. temperatureunder reflux for 3 hours
  7. filtrationfiltered through diatomaceous earth
  8. concentrationThe filtrate was concentrated under reduced pressure