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[ CAS No. 1048025-60-0 ] {[proInfo.proName]}

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Chemical Structure| 1048025-60-0
Chemical Structure| 1048025-60-0
Structure of 1048025-60-0 * Storage: {[proInfo.prStorage]}
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Product Details of [ 1048025-60-0 ]

CAS No. :1048025-60-0 MDL No. :MFCD22381867
Formula : C8H6FIO2 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 280.04 Pubchem ID :-
Synonyms :

Safety of [ 1048025-60-0 ]

Signal Word:Danger Class:6.1
Precautionary Statements:P301+P310 UN#:2811
Hazard Statements:H301 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 1048025-60-0 ]

* 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 [ 1048025-60-0 ]

[ 1048025-60-0 ] Synthesis Path-Downstream   1~4

  • 1
  • [ 321-21-1 ]
  • [ 1048025-60-0 ]
YieldReaction ConditionsOperation in experiment
84% With [bis(acetoxy)iodo]benzene; iodine; palladium diacetate; In N,N-dimethyl-formamide; at 100℃; for 18h;Inert atmosphere; A mixture of <strong>[321-21-1]4-fluoro-2-methyl-benzoic acid</strong> (XII) (20.00 g, 0.130 mol), iodobenzene diacetate (50.15 g, 0.156 mol), iodine (39.52 g, 0.156 mol) and palladium(II) acetate (1.46 g, 0.006 mol) in N,N-dimethylformamide (360 mL) was degassed by cycling vacuum and nitrogen three times and then was heated for 18 h at 100C internal temperature, under argon. The resultant dark mixture was cooled to room temperature, diluted with methyl-tert-butylether (200 mL) and treated with a solution of sodium metabisulfite (250 g) in water (500 mL) under efficient stirring. Then, this yellowcolored mixture was acidified by slowly adding conc. hydrochloric acid (130 mL). The aqueous layer was separated and extracted twice with methyl-tert-butylether (mLlOO x 2). The combined organic extracts were treated with a solution of sodium hydroxide pellets (80 g) in water (300 mL) under stirring. The organic layer containing only iodobenzene was discharged, while the aqueous layer was added with sodium chloride, cooled to ice temperature and brought to very low pH with conc. hydrochloric acid (130 mL). From this aqueous medium the product wasextracted with methyl-tert-butylether (100 mL x 3) and the combined extracts were dried over Na2SO4 and finally concentrated under reduced pressure affording 30.5 g (84%) of 4-fluoro-2-iodo-6-methyl-benzoic acid as brown solid. This raw material was used in the next step without purification.1H NMR (300.0 MHz, CDCI3) 6 ppm 2.46 (s, 3 H), 6.96 (dd, JHF = 9.1, JHH = 2.6 Hz, 1 H), 7.45 (dd, J HF = 7.9, 2.3 Hz,1 H).
69.4% 15.1 4-Fluoro-2-iodo-6-methylbenzoic acid The title compound was prepared in analogy to the process described in Example 14.1 starting from <strong>[321-21-1]4-fluoro-2-methyl benzoic acid</strong>. Yield: 69.4%; LCMS (ESI+): m/z (M+H)+281.7, Rt: 1.952 min.
130 g With [bis(acetoxy)iodo]benzene; iodine; palladium diacetate; In N,N-dimethyl-formamide; at 100℃; for 48h; A solution of <strong>[321-21-1]4-fluoro-2-methylbenzoic acid</strong> (80 g), iodobenzene diacetate (234 g), palladium(II) acetate (5.82 g) and iodine (264 g) in DMF (1000 mL) was stirred at 100C for 2 days. The reaction solution was diluted with saturated aqueous sodium sulfite solution and methyl tert-butyl ether, and the organic layer was separated, washed with 2N sodium hydroxide, and adjusted to pH=3-4 with 1N hydrochloric acid. The organic layer was separated, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by silica gel chromatography (petroleum ether-ethyl acetate) to give the title compound (130 g). 1H NMR (400 MHz, DMSO-d6) delta 2.31 (3H, s), 7.20 (1H, dd, J = 10.0, 2.0 Hz), 7.59 (1H, dd, J = 8.0, 2.4 Hz).
  • 2
  • [ 1048025-60-0 ]
  • [ 877151-43-4 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1.1: potassium carbonate / N,N-dimethyl-formamide / 0.25 h 1.2: 2 h / 20 °C 2.1: N,N-dimethyl-formamide / 5 h / 110 °C
  • 3
  • [ 1048025-60-0 ]
  • [ 80-48-8 ]
  • [ 877151-07-0 ]
YieldReaction ConditionsOperation in experiment
81% To a solution of 4-fluoro-2-iodo-6-methyl-benzoic acid (VII) (30.05 g, 0.109 mol) in N,N-dimethylformamide (300 mL) was added anhydrous potassium carbonate (22.0 g, 0.16 mol) under efficient magnetic stirring. After 15 mm methyl p-toluensulfonate (30.7 g, 0.16 mol) was added. The brown suspension was stirred at room temperature for 2 h.Potassium acetate (12.4 g, 0.13 mol) was then added to destroy the unreacted methyl p-toluensulfonate and the mixture was stirred overnight. The thick reaction mixture was diluted with methyl-tert-butylether (100 mL) and washed with water (600 mL); the aqueous layer was separated and extracted twice with methyl-tert-butylether (70 mL x 2). The combined organic extracts were washed with brine (50 mL), dried over Na2SO4 and concentrated under reduced pressure to a solid residue. This material was purified by chromatography (eluant n-hexane/ethyl acetate 9:1),affording 26.2 g (81%) of product as colorless oil.1H NMR (400.5 MHz, DMSO-d6) ppm 2.27 (s, 3 H), 3.86 (s, 3 H), 7.25 (dd, JHF 9.6, JHH 2.4 Hz, 1 H), 7.63 (dd,JHF = 8.2, JHH = 2.4 Hz, 1 H).
  • 4
  • [ 1048025-60-0 ]
  • [ 74-88-4 ]
  • [ 877151-07-0 ]
YieldReaction ConditionsOperation in experiment
90 g With potassium carbonate; In N,N-dimethyl-formamide; at 20℃; for 16h; A solution of 4-fluoro-2-iodo-6-methylbenzoic acid (130 g) obtained in Reference Example 97, methyl iodide (72.4 g) and potassium carbonate (70.4 g) in DMF (1000 mL) was stirred at room temperature for 16 hr. The reaction solution was diluted with water and ethyl acetate, and the organic layer was separated, washed with water, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by silica gel chromatography (petroleum ether-ethyl acetate) to give the title compound (90 g). 1H NMR (400 MHz, CDCl3) delta 2.34 (3H, s), 3.94 (3H, s), 6.85-7.00 (1H, m), 7.33-7.45 (1H, m).
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