反应详情

Add 2-methyl-5-(2-nitrovinyl)thiophene (483 mg crude, 2.855 mmol, 1 eq) as a solution in diethyl ether (15 mL) to a solution of lithium aluminum hydride (227 mg, 5.995 mmol, 2.1 eq) in diethyl ether (5.995 mL) at a rate such as to maintain gentle reflux of the solution. Stir reaction for 5 minutes. Cautiously add water followed by several small portions of potassium sodium tartrate. Stir reaction vigorously for 1 hour and then let stand overnight. Separate organics, dry with magnesium sulfate, and concentrate on rotovap to give 360 mg of crude product as an oil. Perform column chromatography to give 82 mg (20% yield) of 2-(5-methylthiophen-2-yl)ethylamine. MS (m/e): 142.0 (MH+).

1. temperatureto maintain gentle
2. temperaturereflux of the solution
3. customreaction for 5 minutes
4. stirringStir
5. customreaction vigorously for 1 hour
6. dry with materialSeparate organics, dry with magnesium sulfate
7. concentrationconcentrate on rotovap
8. customto give 360 mg of crude product as an oil