Carbon Dioxide → HCID 20069236, compound
Reaction equation
C(=O)=O.[Na].[CH3:5][C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[CH2:7].CO.O1[CH2:20][CH2:19][CH2:18][CH2:17]1>>[CH:9]1[C:10]2[C:11](=[CH:17][C:18]3[C:8]([CH:9]=2)=[CH:6][CH:5]=[CH:20][CH:19]=3)[CH:12]=[CH:13][C:8]=1[C:6]([CH3:5])=[CH2:7]Participants
Conditions
- Temperature
- -40 °C
Procedure
About 100 milliliters of tetrahydrofuran is vacuum distilled into a light tight ampule containing the above monomer, the ampule chilled to the temperature of dry ice (approximately -40° C) and about 5 milliliters of initiator solution (5 × 10-5 moles of the sodium salt of alphamethyl styrene tetramer in tetrahydrofuran) injected into the ampule through a side arm on the ampule. Polymerization of the monomer commences upon the introduction of the initiator into the ampule. After about 24 hours of continuous stirring at -40° C, the contents of the ampule are emptied into a flask containing methanol thereby quenching the polymerization reaction and precipitating the polymer. The polymer solids are recovered from the methanol solution by filtration, dried and reprecipitated from benzene with methanol. Yield: 8.0 grams of white polymer, Mw 280,000, Mw /Mn 1.74.
Workup
- distillationdistilled into a light tight ampule
- additioncontaining the above monomer
- customPolymerization of the monomer commences upon the introduction of the initiator into the ampule
- customthe contents of the ampule are emptied into a flask
- customthereby quenching
- customthe polymerization reaction
- customprecipitating the polymer
- filtrationThe polymer solids are recovered from the methanol solution by filtration
- customdried
- customreprecipitated from benzene with methanol
Sources & evidence
- ORD record
- ord-b406ce054fa045358c19731ed9b5cb3e
- Source dataset
- uspto-grants-1978_09
- Patent number
- US04117239
Reaction notes
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