反应详情

温度

75 °C

1.6 ml (15 mmol.) of TMEDA are added to 1.93 g (10 mmol.) of 1 in 30 ml of hexane. A solution (1.6 M in hexane) of n-BuLi (6.25 ml, 10 mmol.) is added dropwise. After 3 hours, reflux (75° C.), the colour has deepened from yellow to orange. Without cooling, a solution of 2.2 ml (10 mmol.) of chlorodicyclohexylphosphane in 20 ml of hexane is added dropwise. Refluxing is carried out for a further one hour, the colour of the mixture lightening again and a white solid precipitating. After cooling, 30 ml of water are added to the mixture. The aqueous phase is extracted 3 times using 20 ml of hexane each time. The combined organic phases are washed with 10 ml of water, dried over Na2SO4 and concentrated in vacuo (45° C.). The yellow residue is boiled for 30 minutes in 30 ml of MeOH. After cooling to RT, the resulting product is filtered off (660 mg, 17%).

1. temperatureWithout cooling
2. temperatureRefluxing
3. waitis carried out for a further one hour
4. customthe colour of the mixture lightening again and a white solid precipitating
5. temperatureAfter cooling
6. addition30 ml of water are added to the mixture
7. extractionThe aqueous phase is extracted 3 times
8. washThe combined organic phases are washed with 10 ml of water
9. dry with materialdried over Na2SO4
10. concentrationconcentrated in vacuo (45° C.)
11. waitThe yellow residue is boiled for 30 minutes in 30 ml of MeOH
12. temperatureAfter cooling to RT
13. filtrationthe resulting product is filtered off (660 mg, 17%)