反应详情

The procedure of Example 10 was repeated except that: 1274 g (≈1.5 liters, 13.83 mole) of toluene was charged to the reactor (38 ppm residual H2O), which was further made anhydrous by the addition of 0.43 g (6.8 mmole) n-butyllithium. The anhydrous toluene was heated to 76° C., upon reaching the set point temperature, a mixture comprised of 18.17 g (0.162 mole) potassium t-butoxide, 154 g (1.67 mole) toluene and 97.96 g of N,N,N′,N′-tetramethylethylenediamine (TMEDA, 0.843 mole) was charged through the charge vessel and delivered subsurface to the gently agitated (300 rpm) toluene solution. The vessel and line were flushed with a 100 ml aliquot of toluene before charging with 62.98 g n-butyllithium solution (2.0 M, 16.5 wt % in cyclohexane, 0.162 mole). All total (the initial charge, the amount used to form the potassium t-butoxide/TMEDA solution and the amount used to flush the charge lines) 1598 g (17.3 mole) of toluene was charged to the reactor prior to initiating the styrene feed. Styrene, 3604 g (34.60 mole) was fed through the 1/16th inch OD feed line over 187 minutes such that the feed velocity was ≈16 ft/s with a feed rate of 19.27 g/min. The reaction mixture was quenched with 19.47 g (0.324 mole) acetic acid in 100 ml of toluene. An aliquot of the reaction mixture gave the following GPC analysis: Mp: 521, Mn: 546, Mw: 842, Mz: 1184, PD: 1.54, σn=402, nα3=1.798. The workup procedure followed the general workup procedure as in Example 10—Part B, with the following conditions:

1. additionwas charged through the charge vessel
2. customThe vessel and line were flushed with a 100 ml aliquot of toluene
3. additionAll total (the initial charge