反应详情

Di-tert-butylphosphine chloride (34 g, 188.41 mmol) was added to a Schlenk flask followed by diethyl ether (200 ml). The ether solution was cooled in a cold water bath and LiAlH4 (1M in diethyl ether, 100 ml, 100 mmol) was added slowly. This gave a yellow suspension which was allowed to stir at room temperature overnight. The suspension was quenched by the water (50 ml, degassed with nitrogen for 20 minutes). This gave a biphasic solution. The upper (organic layer) was cannula transferred into a clean Schlenk and the aqueous residues washed with a further 100 ml of ether. The ether extracts were combined and dried with sodium sulphate. The ether extracts were then cannula transferred into a clean Schlenk and the ether removed by distillation. This gave a colourless oil. Yield=22.0 g, 80%. 31P {1H} NMR (161.9 MHz, CDCl3): δ 21.0 ppm

1. customThis gave a yellow suspension which
2. customThe suspension was quenched by the water (50 ml, degassed with nitrogen for 20 minutes)
3. customThis gave a biphasic solution
4. customtransferred into a clean Schlenk
5. washthe aqueous residues washed with a further 100 ml of ether
6. dry with materialdried with sodium sulphate
7. customcannula transferred into a clean Schlenk
8. customthe ether removed by distillation
9. customThis gave a colourless oil