反应详情

A suspension of LiAlH4 (4.66 g) in dry Et2O (100 mL) was cooled in an ice bath, and a solution of 2,2-diethyl-malononitrile (5.0 g) in Et2O (50 mL) was added dropwise at such a rate that the temperature was kept below 20° C. The mixture was stirred overnight at room temperature, cooled in an ice bath, and quenched by adding H2O (5 mL), 2M aqueous NaOH (10 mL) and again H2O (5 mL). The suspension was filtered, the filter cake was washed with Et2O, and the combined filtrates were evaporated to dryness under reduced pressure to give 5.0 g of a clear, light-yellow liquid. 1H NMR (400 MHz, CDCl3) δ 0.80 (t, J=8 Hz, 6H), 1.08 (br s, 4H), 1.22 (q, J=8 Hz, 4H), 2.52 (s, 4H).

1. temperaturewas cooled in an ice bath
2. customwas kept below 20° C
3. temperaturecooled in an ice bath
4. customquenched
5. additionby adding H2O (5 mL), 2M aqueous NaOH (10 mL) and again H2O (5 mL)
6. filtrationThe suspension was filtered
7. washthe filter cake was washed with Et2O
8. customthe combined filtrates were evaporated to dryness under reduced pressure
9. customto give 5.0 g of a clear, light-yellow liquid