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温度

0 °C

The nitrile 20C (3.2 g, 12.85 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) and 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 as a yellow oil. The amine was used for the following step without purification.

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