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[ CAS No. 38103-06-9 ]

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Chemical Structure| 38103-06-9
Chemical Structure| 38103-06-9
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CAS No. :38103-06-9 MDL No. :MFCD00319167
Formula : C31H20O8 Boiling Point : 712.3°C at 760 mmHg
Linear Structure Formula :- InChI Key :N/A
M.W :520.49 g/mol Pubchem ID :94483
Synonyms :

Safety of [ 38103-06-9 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P280-P305+P351+P338 UN#:N/A
Hazard Statements:H302-H315-H319-H332-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 38103-06-9 ]

  • Upstream synthesis route of [ 38103-06-9 ]
  • Downstream synthetic route of [ 38103-06-9 ]

[ 38103-06-9 ] Synthesis Path-Upstream   1~7

  • 1
  • [ 80-05-7 ]
  • [ 118-45-6 ]
  • [ 38103-06-9 ]
YieldReaction ConditionsOperation in experiment
85%
Stage #1: With N-benzyl-N,N,N-triethylammonium chloride; sodium hydroxide In water at 85 - 172℃; for 15 h;
Stage #2: at 130 - 145℃; for 5 h;
79 g (0.63 mol) of a 32percent by weight aqueous sodium hydroxide solution and 62.4 g (0.3 mol) of bisphenol A were charged into the reactor.Stir and dissolve,The temperature rises to 85 ° C and the solution is transparent.Next, 510 g of a trimethylbenzene solvent and 4.2 g of a benzyltriethylammonium chloride catalyst were added.Warming and refluxing,The temperature rose to 172 ° C,Stirring reaction for 15 hours,Then cool down to 130 ° C,108 g (0.6 mol) of 4-chlorophthalic anhydride and 4.86 g of benzyltriethylammonium chloride catalyst were added.Heating from 140 ° C to 145 ° C,Reflow reaction for 5 hours,Then filter hot,Pumping the filtrate into the crystallization kettle,The filtrate is cooled to room temperature.Crystallized for 12 hours,filter,The precipitate is washed with ion-free water,Filtration, precipitation was obtained and washed with 250 g of ethanol.Stirring for 2 hours,filter,Get wet material 125g,After drying, 120 g of bisphenol A diether dianhydride product (yield 85percent),The product is white powder,
Reference: [1] Patent: CN108148029, 2018, A, . Location in patent: Paragraph 0011; 0012; 0014
  • 2
  • [ 319-03-9 ]
  • [ 2444-90-8 ]
  • [ 38103-06-9 ]
YieldReaction ConditionsOperation in experiment
90% at 180℃; for 0.25 h; A dry 100 mL flask was charged with 1.69 g (7.3 mmol) of the disodium salt of biphenol, 2.44 g, (146 mmol) of 4-fluorophthalic anhydride, 2 mL (14 mmol) of hexaethylguanidinium chloride as a 15 weight percent solution in o-dichlorobenzene, and 44 g of dry o-dichlorobenzene. The flask was immersed in an oil bath maintained at 180° C. and the mixture was stirred magnetically. After 15 minutes, the reaction mixture was filtered hot to remove the sodium fluoride by-product. The filtrate was allowed to cool to room temperature and the product dianhydride crystallized from the solvent as a cream colored solid which was isolated by filtration (3.1 g, 90percent yield).
82% at 175℃; for 1 h; A dry 25 mL flask was charged with 403 mg (1.482 mmol) of the disodium salt of bisphenol A, 500 mg (3.012 mmol) of 4-fluorophthalic anhydride, 46 mg (0.148 mmol) of 4-(N,N-dibutylamino)-N-neopentylpyridinium chloride, 8.5 g (10percent solids) of dry o-dichlorobenzene and 55 mg of o-terphenyl (internal standard). The flask was immersed in an oil bath maintained at 180° C. and the mixture was stirred magnetically. The temperature within the reaction flask was about 175° C. Samples (0.1 mL) were withdrawn periodically dissolved in 6 mL of acetic acid and approximately. 0.5 mL of methylamine (40percent aqueous soln.) and heated at 125-130° C. for 1.5 hours. These samples were analyzed for the bis N-methyl imide of bisphenol A dianhydride by liquid chromatography. By following the diether dianhydride formation in this manner it was determined that the yield of product bisphenol A dianhydride (BPADA) had reached 82percent after one hour.
Reference: [1] Patent: US2006/205958, 2006, A1, . Location in patent: Page/Page column 6
[2] Patent: US2006/205958, 2006, A1, . Location in patent: Page/Page column 5; 6
  • 3
  • [ 118-45-6 ]
  • [ 2444-90-8 ]
  • [ 38103-06-9 ]
YieldReaction ConditionsOperation in experiment
25% at 180℃; for 5 h; A dry 100 mL flask was charged with 2.0 g (7.3 mmol) of the disodium salt of bisphenol A, 2.67 g (14.6 mmol) of 4-chlorophthalic anhydride, 4 mL (14 mmol) of hexaethylguanidinium chloride as a 15 weight percent solution in o-dichlorobenzene, 48 g of dry o-dichlorobenzene, and 100 mg of o-terphenyl (internal standard). The flask was immersed in an oil bath maintained at 180° C. and the mixture was stirred magnetically. The reaction was followed as in Example 1. The yield of biphenol dianhydride had reached 25percent after 5 hours.
Reference: [1] Patent: US2006/205958, 2006, A1, . Location in patent: Page/Page column 6
  • 4
  • [ 38103-05-8 ]
  • [ 38103-06-9 ]
Reference: [1] Molecular Crystals and Liquid Crystals, 2004, vol. 418, p. 11/[739]-19/[747]
[2] Macromolecules, 2006, vol. 39, # 22, p. 7534 - 7548
  • 5
  • [ 80-05-7 ]
  • [ 38103-06-9 ]
Reference: [1] Macromolecules, 2006, vol. 39, # 22, p. 7534 - 7548
[2] Molecular Crystals and Liquid Crystals, 2004, vol. 418, p. 11/[739]-19/[747]
  • 6
  • [ 31643-49-9 ]
  • [ 38103-06-9 ]
Reference: [1] Macromolecules, 2006, vol. 39, # 22, p. 7534 - 7548
[2] Molecular Crystals and Liquid Crystals, 2004, vol. 418, p. 11/[739]-19/[747]
  • 7
  • [ 38791-67-2 ]
  • [ 38103-06-9 ]
Reference: [1] Macromolecules, 2006, vol. 39, # 22, p. 7534 - 7548
[2] Molecular Crystals and Liquid Crystals, 2004, vol. 418, p. 11/[739]-19/[747]
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