HRID1720067
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturea cooled
- temperatureThe mixture was heated
- temperatureat reflux for 45 min
- customExcess LiAIH4 was destroyed by successive addition of H2O (0.15 ml), 15% NaOH (0.15 ml) and H2O (0.4 ml)
- customThe white precipitate was removed by filtration
- washwashed with THF (10 ml)
- dry with materialAfter drying (MgSO4)
- customthe flitrate was evaporated under reduced pressure