1.6 ml (15 mmol) of TMEDA was added to 1.93 g (10 mmol) dissolved in 30 ml of hexanes within 1 . A solution of n-BuLi (6.25 ml, 10 mmol) (concentration 1.6 M in hexane) was added dropwise. after 3 hr reflux (75C), the color deepened from yellow to orange. Without cooling, 2.2 ml (10 mmol) of a solution of chlorinated di-tert-butylphosphine in 20 ml hexane was added dropwise. Refluxing was carried out for another hour, and the color of the mixture was again lightened and a white solid precipitated. After cooling, 30 ml of water was added to the mixture. Three extractions of the aqueous phase were carried out, each using 20 ml of hexane. The combined organic phases were washed with 10 ml of water, dried over Na2SO4 and concentrated under vacuum (45C). The yellow residue was boiled in 30 ml of MeOH for 30 min. After cooling to room temperature, the resulting product (660 mg, 17%) was filtered.
