Oxygen → HCID 178506801, compound

HRID 2084570Notes

Reaction equation

C([Li:5])(CC)C.O=O.[C:8]1([C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH2:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[CH2:22]1CC[CH2:25][CH2:24][CH2:23]1>>[C:8]1([C:14]([Li:5])([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:15][CH2:22][CH2:23][CH2:24][CH3:25])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

Participants

Reactant 4

HCID 977Oxygen

HCID 8078Cyclohexane

HCID 107401,1-Diphenylethylene

HCID 178418400CID 53628100

Product 1

HCID 178506801HCID 178506801, compound

Procedure

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).

Workup

customAn initiator slurry was prepared

Sources & evidence

ORD record: ord-4ca4c1a3b25844e5820e74694e67392e
Source dataset: uspto-grants-2004_04
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06716935B1

Reaction notes

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