9,9-Bis(4-hydroxyphenyl)fluorene → HCID 131730505, compound

HRID 1889615Notes

Reaction equation

HRID 1889615 reaction equation
[CH3:1][O:2]CC1C=CC(COC)=CC=1.[Cl-].[Al+3].[Cl-].[Cl-].C1C2[C:28](C3C=CC(O)=CC=3)([C:30]3C=[CH:34][C:33]([OH:36])=[CH:32][CH:31]=3)[C:27]3C(=CC=CC=3)C=2C=CC=1>C1(=O)OCCC1>[CH3:34][C:33]([CH2:32][CH2:31][CH2:30][CH2:28][CH3:27])=[O:36].[CH3:1][OH:2]

Participants

5

Reactant 3

HCID 767169,9-Bis(4-hydroxyphenyl)fluoreneHCID 812391,4-Bis(Methoxymethyl)BenzeneHCID 6451240Aluminum(III) Chloride

Product 1

HCID 131730505HCID 131730505, compound

Reagents, catalysts & solvents 1

HCID 7302Gamma-ButyrolactoneSolvent2×

Procedure

8.75 g (0.05 mol) of α,α′-dimethoxy-p-xylene, 26.66 g of aluminum chloride, and 200 g of γ-butyrolactone are introduced into a 1 l 4-neck flask mounted with a mechanical stirrer, a condenser, a 300 ml dropping funnel, and a nitrogen gas-introduction tube with inflowing nitrogen gas, and sufficiently stirred. After 10 minutes, a solution in which 35.03 g (0.10 mol) of 4,4′-(9-fluorenylidene)diphenol is dissolved in 200 g of γ-butyrolactone is slowly dripped for 30 minutes and reacted for 12 hours. After completing the reaction, the acid is removed using water and condensed by an evaporator. Then it is diluted using methylamylketone (MAK) and methanol to provide a solution of MAK/methanol=4/1 (weight ratio) in a concentration of 15 wt %. The solution is introduced into a 31 separate funnel and added with n-heptane to remove a low molecular body including a monomer. A polymer (Mw=10,000, polydispersity=2.0) represented by the following Chemical Formula 1A is provided.

Workup

  1. custommounted with a mechanical stirrer, a condenser
  2. waitis slowly dripped for 30 minutes
  3. customreacted for 12 hours
  4. customthe reaction
  5. customthe acid is removed
  6. customwater and condensed
  7. customby an evaporator
  8. additionThen it is diluted

Sources & evidence

ORD record
ord-7e6c8edb8a694d679c3bebb7a70b1257
Source dataset
uspto-grants-2013_08
Patent number
US08502334B2

Reaction notes

Loading…