反应详情

温度

-25 °C

A Grignard mixture of 55 mmoles of cyclohexylmagnesium chloride (prepared from 1.5 g of magnesium turnings and 6.5 g of cyclohexylchloride in 20 ml of anhydrous ether) was added dropwise to a stirred solution of 8.9 g (50 mmoles) of phenyldichlorophosphine in 50 ml of anhydrous ether maintained under an inert atmosphere at -25° C. After the addition was complete, the resulting mixture was allowed to gradually warm to ambient temperature and then was refluxed for 15 minutes. The stirred mixture was cooled and a solution of 75 mmoles of isopropylmagnesium bromide (prepared from 2.1 g of magnesium turnings and 9.5 g of isopropyl bromide in 29 ml of anhydrous ether) was added dropwise at temperatures between 0° C. and +30° C. After refluxing for 4 hours, the reaction mixture was cooled to 0° C. and treated dropwise with 25 ml of water, thereby giving two phases. The ether phase was separated, dried over magnesium sulfate, concentrated, and distilled to give cyclohexylisopropylphenylphosphine: 31P-NMR δ=6.08 ppm; boiling point ("BP")=104°-105° C. at 0.05 torr, Chemical Ionization Mass Spec [M+H+ =235, yield=about 67%.

1. additionAfter the addition
2. temperatureto gradually warm to ambient temperature
3. temperaturewas refluxed for 15 minutes
4. temperatureThe stirred mixture was cooled
5. temperatureAfter refluxing for 4 hours
6. temperaturethe reaction mixture was cooled to 0° C.
7. customgiving two phases
8. customThe ether phase was separated
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated
11. distillationdistilled