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[ CAS No. 861905-21-7 ] {[proInfo.proName]}

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Chemical Structure| 861905-21-7
Chemical Structure| 861905-21-7
Structure of 861905-21-7 * Storage: {[proInfo.prStorage]}
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Product Details of [ 861905-21-7 ]

CAS No. :861905-21-7 MDL No. :MFCD24107118
Formula : C9H8FIO2 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 294.06 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 861905-21-7 ]

* 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 [ 861905-21-7 ]

[ 861905-21-7 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 67-56-1 ]
  • [ 861905-94-4 ]
  • [ 861905-21-7 ]
YieldReaction ConditionsOperation in experiment
100% With sulfuric acid In water at 20 - 50℃; for 15h; 1.3 Preparation of methyl 3-fluoro-5-iodo-4-methylbenzoate; 3-Fluoro-5-iodo-4-methylbenzoic acid (1 eqv) was dissolved in methanol (6.6 vol) and treated with 98% sulphuric acid (0.375 vol) at 2O0C. The solution was heated to 50°C and stirred for 15h at this temperature then the solution cooled to 20°C.The volume of the solution was reduced to 25% of the initial volume by vacuum distillation. After cooling to 2O0C, TBME (5.5 vol) was added, followed by 8% aqueous NaHCO3 solution (9.4 vol) over 15 min to a pH of 7-8. After stirring for 10 min, the layers were separated and the aqueous layer was extracted with further TBME (5.5 vol). After stirring for 10 min, the layers were separated and the combined organic layers were stirred and washed with water (4.6 vol). After stirring for 10 min, the layers were separated and the organic layer was concentrated and dried at 45 - 500C to give the title compound. Yield: ca. 100% th.
77% With sulfuric acid at 50℃; Inert atmosphere; Large scale;
With sulfuric acid for 6h; Heating / reflux; A stirred mixture of 3-fluoro-4-methylbenzoic acid (10.3g) in trifluoromethane sulfonic acid (50ml) at -20°C was treated with N-iodosuccinimide in portions over 40min. The reaction was stirred at -10°C for 44h when a further amount of N-iodosuccinimide (6.0g) was added. After 20h the reaction mixture was added to ice/water and extracted with ethyl acetate. The organic solution was washed with aqueous sodium metabisulfite and dried over sodium sulfate. The residue was dissolved in methanol (50ml), the solution was treated with concentrated sulfuric acid (91ml) and the mixture was heated at reflux for 6h. The solvent was evaporated and the residue was dissolved in ethyl acetate. This solution was washed with aqueous sodium bicarbonate and dried with brine and over magnesium sulfate. Purification by biotage chromatography (x2), firstly using cyclohexane/ethyl acetate (100/1) and secondly cyclohexane/toluene (6/1) as eluents gave the title compound (9.31 g). LC-MS: Rt 3.55min.
  • 2
  • [ 861905-94-4 ]
  • [ 861905-21-7 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1: thionyl chloride / 1.75 - 3 h / 95 °C / Heating / reflux 2: triethylamine / dichloromethane / 0 - 20 °C
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