反应详情

温度

0 °C

The nitrile 28A (4.7 g, 12 mmol) dissolved in 50 ml of diethyl ether was added dropwise to a mixture of LiAlH4 (912 mg, 2 equiv.) in diethyl ether (80 mL) stirred at 0° C. Then the mixture was stirred at room temperature overnight. The excess of LiAlH4 was destroyed by water addition at 0° C., the solid formed was filtered, washed with Et2O and the filtrate was dried over Na2SO4 and evaporated to dryness to obtain 2.5 g of the amine 29A as yellow solid. Yield=52% 1HNMR (DMSO, 400 MHz) δ 2.25 (2H, bs), 3.90 (2H, s), 7.90 (4H, d, J=8 Hz), 8.11 (2H, s), 8.40 (4H, d, J=8 Hz)

1. stirringThen the mixture was stirred at room temperature overnight
2. customThe excess of LiAlH4 was destroyed by water addition at 0° C.
3. customthe solid formed
4. filtrationwas filtered
5. washwashed with Et2O
6. dry with materialthe filtrate was dried over Na2SO4
7. customevaporated to dryness