Water → Phthalic Anhydride

HRID 718474Notes

Reaction equation

HRID 718474 reaction equation
Cl[C:2]1[CH:12]=[CH:11][CH:10]=[C:4]2[C:5]([O:7][C:8](=[O:9])[C:3]=12)=[O:6].O>C1C=CC(Cl)=C(Cl)C=1>[C:8]1(=[O:9])[O:7][C:5](=[O:6])[C:4]2=[CH:10][CH:11]=[CH:12][CH:2]=[C:3]12

Participants

4

Reactant 2

HCID 962WaterHCID 670143-Chlorophthalic anhydride

Product 1

HCID 6811Phthalic Anhydride

Reagents, catalysts & solvents 1

HCID 72391,2-DichlorobenzeneSolvent

Procedure

In the “In Situ ClPAMI” procedure, the five-necked flask setup described above was used. The ClPAMI was synthesized in the five-necked flask by reacting two moles of chlorophthalic anhydride with one mole of mPD using oDCB as solvent. The water formed was removed by distillation until a moisture content of less than 20 ppm in the distillate was obtained. Then, HEGCl, a phase transfer catalyst, was added in an amount of 0.6 weight %, based on the ClPAMI amount. More oDCB was distilled off to confirm that the moisture level was less than 20 ppm in the distillate. Then, a slurry of Na2BPA and NaPCP in oDCB in the second flask was transferred to the five-necked flask using the addition tube in communication with the second flask, and polymerization was conducted at 180° C.

Workup

  1. customThe ClPAMI was synthesized in the five-necked flask
  2. customwas removed by distillation until a moisture content of less than 20 ppm in the distillate
  3. customwas obtained
  4. additionThen, HEGCl, a phase transfer catalyst, was added in an amount of 0.6 weight %
  5. distillationMore oDCB was distilled off
  6. customwith the second flask, and polymerization
  7. customwas conducted at 180° C.

Sources & evidence

ORD record
ord-8d2255d7360c4be6a71cde849149c034
Source dataset
uspto-grants-2015_11
Patent number
US09193829B2

Reaction notes

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