Methanol → 4-Vinylphenol
Reaction equation
C[OH:2].S(OOS([O-])(=O)=O)([O-])(=O)=O.[K+].[K+].[CH2:15]=[CH:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C=CC=C>O.Cl>[CH2:15]=[CH:16][C:17]1[CH:22]=[CH:21][C:20]([OH:2])=[CH:19][CH:18]=1Participants
Reactant 4
Product 1
Reagents, catalysts & solvents 2
Procedure
483 g of the methanol solution from Ex. 5 were stripped of the solvent and the residue dissolved in 1300 ml of RO water containing 118 g of conc. hydrochloric acid to prepare a 9.9 percent aq. solution of the protonated water-soluble poly(4-vinylpyridine) RAFT macroinitiator. One gram of potassium persulfate was then dissolved in 252.5 g of the 9.9 percent aq. macroinitiator solution (˜25 g polymer). This solution was then charged into a one quart heavy-walled bottle preflushed with nitrogen, followed by the addition of 60.0 g (0.577 moles) of styrene and 90.0 g (˜1.67 moles) of butadiene. The bottle was then capped and tumbled in a 65° C. water bath. The progress of the reaction was monitored gravimetrically by periodically sampling solids content by means of a syringe needle through a gasketed hole in the metal cap. After 23 hrs., the bottle was removed from the bath and cooled to room temperature to stop polymerization. The solids content was determined to be 32.3 percent or ˜70 percent conversion of the styrene and butadiene.
Workup
- additionThis solution was then charged into a one quart heavy-walled bottle
- customThe bottle was then capped
- customtumbled in a 65° C.
- aliquotby periodically sampling solids content by means of a syringe needle through a gasketed hole in the metal
- customcap
- custom, the bottle was removed from the bath
- custompolymerization
Sources & evidence
- ORD record
- ord-97e34be40b4d4b5fbd8155e72e70b239
- Source dataset
- uspto-grants-2009_12
- Patent number
- US07625985B1
Reaction notes
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