HRID1720067

反应详情

EQUATION

反应方程式

HRID 1720067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the 5-benzyl-3-(2-nitroethenyl)indole (0.1 g, 0.4 mmol)in dry THF was added dropwise to a cooled (ice bath) suspension of LiAIH4 (0.1 g, 2.4 mmol)in 5 ml of dry THF under nitrogen. The mixture was heated at reflux for 45 min. Excess LiAIH4 was destroyed by successive addition of H2O (0.15 ml), 15% NaOH (0.15 ml) and H2O (0.4 ml). The white precipitate was removed by filtration and washed with THF (10 ml). After drying (MgSO4), the flitrate was evaporated under reduced pressure to give 0.04 g (45%) of 3-(2-aminoethyl)-5-benzylindole as a free base. The free base was converted to the fumarate salt, mp 150°-153° C.

WORKUP

后处理

  1. temperaturea cooled
  2. temperatureThe mixture was heated
  3. temperatureat reflux for 45 min
  4. customExcess LiAIH4 was destroyed by successive addition of H2O (0.15 ml), 15% NaOH (0.15 ml) and H2O (0.4 ml)
  5. customThe white precipitate was removed by filtration
  6. washwashed with THF (10 ml)
  7. dry with materialAfter drying (MgSO4)
  8. customthe flitrate was evaporated under reduced pressure