反应详情

温度

0 °C

The nitrile 26D (2 g, 5.7 mmol) dissolved in 50 ml of diethyl ether was added dropwise to a mixture of LiAlH4 (434 mg, 2 equiv.) in diethyl ether (60 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 1.3 g of the amine 27D as a yellow oil. Yield=65% 1HNMR (DMSO, 400 MHz) δ 3.30 (2H, bs), 3.51 (4H, m), 3.76 (6H, m), 6.80 (1H, s), 7.29 (1H, s), 7.42 (2H, d, J=8 Hz), 8.18 (2H, dd)

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