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Product Details of [ 22433-91-6 ]

CAS No. :22433-91-6 MDL No. :MFCD00099229
Formula : C8H5BrO4 Boiling Point : -
Linear Structure Formula :- InChI Key :LOICBODWTPYJIW-UHFFFAOYSA-N
M.W : 245.03 Pubchem ID :329530
Synonyms :

Safety of [ 22433-91-6 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313 UN#:N/A
Hazard Statements:H315-H319 Packing Group:N/A
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Application In Synthesis of [ 22433-91-6 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Upstream synthesis route of [ 22433-91-6 ]
  • Downstream synthetic route of [ 22433-91-6 ]

[ 22433-91-6 ] Synthesis Path-Upstream   1~2

  • 1
  • [ 67-56-1 ]
  • [ 22433-91-6 ]
  • [ 39622-80-5 ]
YieldReaction ConditionsOperation in experiment
99.7%
Stage #1: for 6 h; Reflux
Stage #2: at 0 - 20℃; for 2.5 h;
2), 2-bromo-1,3-phthalic acid (2) (17.9 g, 73.1 mmol) was dissolved in thionyl chloride (100 mL) and heated to refluxAfter 6 h spin dry under vacuum.A mixed solution of methanol (80 mL) and triethylamine (40 mL) was added dropwise to the residue at 0 ° C,Dropping 0.5h.After stirring at room temperature for 2 h,Concentrated under vacuum.The residue was dissolved in ethyl acetate,With 0.5M hydrochloric acid aqueous solution and saturated sodium bicarbonate once washed,The organic phase was dried over anhydrous sodium sulfate,Dried under vacuum to give dimethyl 2-bromo-1,3-phthalic acid as a yellow oil (3) (19.9 g, 99.7percent).
95.5%
Stage #1: at 100℃; for 9 h;
Stage #2: at 20 - 25℃; for 2 h;
2-Bromo-l, 3-benzenedicarboxylic acid (44.20 g, 180.4 mmol) in SOCl2 (300 mL) was gradually heated to 100 0C during a period of 5 h and stirred at 100 0C for another 4 h. After SOCl2 was evaporated in vacuo and the flask was cooled to 0 0C, methanol (200 mL) and triethylamine (100 mL) were added slowly while stirring. The reaction mixture was stirred at room temperature for 2 h and was concentrated in vacuo. The residue was extracted with EtOAc, dried over MgSO4 and concentrated in vacuo to obtain 47.05 g of the title compound (95.5percent). 1H NMR (400 MHz, CDCl3): δ 7.70 (m, 2H), 7.40 (t, IH), 3.94 (s, 6H); 13C NMR (100 MHz, CDCl3): δ 166.0, 134.8, 132.0, 126.9, 117.9, 52.5; HRMS-ES: Ci0H9BrO4 calcd 241.9684, found 241.9683.
Reference: [1] Patent: CN107090000, 2017, A, . Location in patent: Paragraph 0031; 0034
[2] Patent: WO2011/22337, 2011, A1, . Location in patent: Page/Page column 66
[3] Journal of the American Chemical Society, 2016, vol. 138, # 2, p. 479 - 482
[4] Journal of Organic Chemistry, 1992, vol. 57, # 18, p. 4940 - 4948
[5] Journal of Biomolecular Structure and Dynamics, 2015, vol. 33, # 9, p. 1899 - 1912
[6] Bioorganic and Medicinal Chemistry Letters, 2017, vol. 27, # 3, p. 537 - 541
[7] Helvetica Chimica Acta, 1972, vol. 55, p. 2599 - 2611
[8] Organic Letters, 2006, vol. 8, # 25, p. 5841 - 5844
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  • [ 22433-91-6 ]
  • [ 79839-49-9 ]
Reference: [1] Patent: WO2011/22337, 2011, A1,
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