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[ CAS No. 1272528-60-5 ] {[proInfo.proName]}

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Chemical Structure| 1272528-60-5
Chemical Structure| 1272528-60-5
Structure of 1272528-60-5 * Storage: {[proInfo.prStorage]}
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Product Details of [ 1272528-60-5 ]

CAS No. :1272528-60-5 MDL No. :MFCD28751453
Formula : C8H8ClIO2 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 298.51 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 1272528-60-5 ]

* 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.

  • Downstream synthetic route of [ 1272528-60-5 ]

[ 1272528-60-5 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 226419-21-2 ]
  • [ 1272528-60-5 ]
YieldReaction ConditionsOperation in experiment
67% Step (ii): 2-Chloro-5-iodo-1 ,3-dimethoxybenzene (3)4-Chloro-3,5-dimethoxyaniline (2) (6.61 g, 35.2 mmol) was added to a mixture of sulfuric acid (9.39 mL, 176 mmol) and H20 (100 mL) at 0C. Sodium nitrite (3.16 g, 45.8 mmol) was added and the reaction mixture was stirred at 0C for 30 min. The mixture was added to a pre-warmed mixture of sodium iodide (21.1 g, 141 mmol), iodine (4.47 g, 17.6 mmol), sulphuric acid (8 mL) and H20 (100 mL) at 80C and the resulting mixture was heated at reflux for 30 min. The mixture was allowed to cool to RT and then 40% sodium thiosulfate solution (200 mL) was added. The product was extracted with EtOAc (300 mL), the solvent was removed in vacuo and the residue was purified by silica gel chromatography (120 g, 0-50% EtOAc in isohexanes) to afford 2-chloro-5-iodo-1 ,3-dimethoxybenzene (3) (7.16 g, 67 % yield).
67% 4-Chloro-3,5-dimethoxyaniline (2) (6.61 g, 35.2 mmol) was added to a mixture of sulfuric acid (9.39 mL, 176 mmol) and H2O (100 mL) at 0 C. Sodium nitrite (3.16 g, 45.8 mmol) was added and the reaction mixture was stirred at 0 C. for 30 min. The mixture was added to a pre-warmed mixture of sodium iodide (21.1 g, 141 mmol), iodine (4.47 g, 17.6 mmol), sulphuric acid (8 mL) and H2O (100 mL) at 80 C. and the resulting mixture was heated at reflux for 30 min. The mixture was allowed to cool to RT and then 40% sodium thiosulfate solution (200 mL) was added. The product was extracted with EtOAc (300 mL), the solvent was removed in vacuo and the residue was purified by silica gel chromatography (120 g, 0-50% EtOAc in isohexanes) to afford 2-chloro-5-iodo-1,3-dimethoxybenzene (3) (7.16 g, 67% yield).
To a solution of <strong>[226419-21-2]4-chloro-3,5-dimethoxyaniline</strong> (2.0 g, 10.70 mmol) in H20 (30 mL) and con. H2504 (3.0 mL)was added the solution of NaNO2 (1.11 g, 16.04 mmol) in water (6.0 mL) at 0-5C, the reaction was stirred at 0-5C for about 30 mm, the solution was added to the pre-warmed mixture of KI (7.11 g, 42.80 mmol) and 12 (1.36 g, 5.35 mmol) in H20 (30 mL) and con. H2504 (3.0 mL) at 80 C, the resulting mixture was stirred at 80 C for about 30 mm. The reaction was allowed to cool to ambient temperature, sat. Na25203 (100 mL) was added to quench the reaction. The mixture was extracted with EA (30 mL x 3), the combined organic phases were washed with sat. NaC1 (20 mL), dried over anhydrous Na2504, filtered, concentrated and purified by column chromatography on silica gel (200-300 mesh, eluent: PE:EA= 10: 1)to give the product as a white solid (2.1 g, 65.9%). ?H NMR (400 IVIFIz, DMSOd6) 7.09 (s, 2H), 3.84 (s, 6H). MS (ESI) m/e [M+1] 298.9.
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