Oxygen → HCID 178506801, compound

Participants

Reaction Steps

An initiator slurry was prepared by mixing 780 ml of 1.3 M sec-butyl lithium in cyclohexane with 8000 g of oxygen-free cyclohexane and stirred at room temperature for about 30 minutes. To this solution was added 197 g of 1,1-diphenylethylene, which resulted in the formation of a red colored solution of 1,1-diphenylhexyl lithium. A 1 wt % solution of 1,6-hexanediol dimethacrylate (HDDMA) was made by pre-dissolving 40 g of HDDMA in 4000 g of purified cyclohexane. The initiator solution was introduced by peristaltic pump at a rate of 24 ml/min into zone 1 of the 3.3 Liter STR along with a 1.0 M solution of triisobutyl aluminum (pressure fed at 4.5 g/min). Purified 2-ethylhexyl methacrylate (EHMA), t-butyl methacrylate (t-BMA) and HDDMA streams were delivered via a reciprocating piston pump at various rates and to various locations of the STR, depending upon the targeted architecture (see Table 3).

Provenance & Evidence