反应详情

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0 °C

A solution of nitrile 20B (3 g, 11.3 mmol) in diethyl ether (30 mL) was added in small amounts to a mixture of LiAlH4 (0.9 g, 2 mol eq) in diethyl ether (35 mL) and stirred at 0° C. After the addition was completed, the mixture was stirred at room temperature overnight. The excess of LiAlH4 was destroyed at 0° C. by addition of small amount of water (30 mL), the solid formed was filtered off and the organic filtrate separated, washed with brine (50 mL) and dried over Na2SO4. The organic phase was evaporated under reduced pressure to obtain 21B as a yellow oil (3.1 g, quantitative yield). 1HNMR (DMSO, 200 MHz) δ 308 (s, 2H), 3.8 (bs, 2H), 7.33 (dd, 1H, J=1.8), 7.47 (dd, 2H, J=2), 7.96 (s, 1H), 8.20 (dd, 2H, J=1.8), 8.57 (dd, 1H, J=1.2).

1. additionAfter the addition
2. stirringthe mixture was stirred at room temperature overnight
3. customThe excess of LiAlH4 was destroyed at 0° C. by addition of small amount of water (30 mL)
4. customthe solid formed
5. filtrationwas filtered off
6. customthe organic filtrate separated
7. washwashed with brine (50 mL)
8. dry with materialdried over Na2SO4
9. customThe organic phase was evaporated under reduced pressure