Vinyl caprolactam → Vcl VP
Reaction equation
[CH:1]([CH:3]1[CH2:10][CH2:9][CH2:8][CH2:7][NH:6][C:4]1=[O:5])=[CH2:2]>C(O)(C)C>[CH:1]([CH:3]1[CH2:10][CH2:9][CH2:8][CH2:7][NH:6][C:4]1=[O:5])=[CH2:2].[CH:7]([N:6]1[CH2:9][CH2:10][CH2:3][C:4]1=[O:5])=[CH2:8]Participants
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
630 g. of isopropanol was charged into a 1-liter resin kettle fitted with a propeller agitator, a reflux condenser, a nitrogen inlet tube, and a thermowatch. The reactor was heated to 82° C. and maintained at this temperature throughout the experiment. A monomer premix was prepared by mixing 52.50 g of vinyl caprolactam, 17.50 g of vinyl pyrrolidone and 1.40 g of t-amyl peroxy-2-ethylhexanoate initiator (Lupersol 575, 95% liquid; Elf Atochem) in a 250-ml beaker. The monomer pre-mix was pumped into the kettle over a period of 2 hours. The reaction then was held at 82° C. for 1 hour. Thereafter 0.50 g of t-amyl peroxy-2-ethylhexanoate was added and the reaction was held 82° C. for 1 hour. The step was repeated twice. At the end of the reaction, a 10% light-brown, viscous poly(vinyl caprolactam) in isopropanol was obtained after cooling to room temperature. Residual vinyl caprolactam was 0.21% by GC analysis. The polymer had a relative viscosity of 1.084 (1% in isopropanol), a GPC molecular weight of 2,640 (polyethylene glycol standard). Dry VCL/VP (75/25) copolymer powder was obtained by vacuum stripping.
Sources & evidence
- ORD record
- ord-3898aca40863495eb0e42fffc39de3f7
- Source dataset
- uspto-grants-2000_09
- Patent number
- US06117929
Reaction notes
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