Dichloromethane → HCID 86587455, compound
Reaction equation
[CH:1]1[CH2:5][CH2:4][CH2:3][CH:2]=1.[CH2:6](Cl)Cl>[Pd]>[CH:1]1[CH2:5][CH2:4][CH2:3][CH:2]=1.[CH3:6][CH:1]1[CH2:5][CH2:4][CH:3]=[CH:2]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Inside a nitrogen purged drybox, the palladium catalyst, {[ (2,6-iPr2Ph)2DABMe2]Pd(CH2CH2CH2CO2Me)}BAF (77 mg, 0.053 mmol) was dissolved in CH2Cl2 (2 ml) and cyclopentene (2 ml) and 3-MeCyp (1 ml) added. The solution was stirred for 4 days after which the volatiles were removed. MeOH was added and the polymer filtered, washed well with MeOH and finally with 2% Irganox® 1010/acetone solution and dried. Yield=1.06 g. Tm (DSC)=210.5° C., Tg (DSC)=73° C. 13C-NMR (TCB, 120° C.) indicated 5% 3-MeCyp incorporation.
Workup
- customwere removed
- additionMeOH was added
- filtrationthe polymer filtered
- washwashed well with MeOH and finally with 2% Irganox® 1010/acetone solution
- customdried
- customTm (DSC)=210.5° C., Tg (DSC)=73° C
- custom13C-NMR (TCB, 120° C.)
Sources & evidence
- ORD record
- ord-a4ff3cb89ea347a59717525237ec0c8e
- Source dataset
- uspto-grants-2001_07
- Patent number
- US06258908B1
Reaction notes
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