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Chemical Structure| 863111-55-1 Chemical Structure| 863111-55-1

Structure of 863111-55-1

Chemical Structure| 863111-55-1

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Product Details of [ 863111-55-1 ]

CAS No. :863111-55-1
Formula : C8H6F3I
M.W : 286.03
SMILES Code : FC(F)(F)C1=CC=CC(I)=C1C
MDL No. :MFCD09800791

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Application In Synthesis of [ 863111-55-1 ]

* 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 [ 863111-55-1 ]

[ 863111-55-1 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 54396-44-0 ]
  • [ 863111-55-1 ]
YieldReaction ConditionsOperation in experiment
73% 3-Amino-2-methylbenzotrifluoride (Aldrich Co., 5.25 g) was added to a mixture of concentrated hydrochloric acid (20 ml) and water (20 ml) and, under ice-cooling, sodium nitrite (3.31 g) dissolved in water (10 ml) was added dropwise thereto. The mixture was stirred at 0°C for 1 hr. Potassium iodide (9.95 g) dissolved in water (20 ml) was added to the reaction mixture. The mixture was stirred at -4°C for 2 hr. The mixture was adjusted to pH 11 or above with a 6N aqueous sodium hydroxide solution, and an aqueous thiosodium sulfate solution was added thereto. The mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried. The solvent was evaporated under reduced pressure to give a brown oil. The oil was purified by silica gel column chromatography (elution solvent: hexane) to give 3-iodo-2-methylbenzotrifluoride (6.28 g, yield 73percent). 1H-NMR(400MHz,DMSO-d6)delta(ppm): 2.52 (3H,s), 7.16(1H,t,J=7.8Hz), 7.73(1H,d,J=7.8Hz), 8.18(1H,d,J=7.8Hz). By a similar operation as in Starting Material Synthetic Example 59, 4-[2-methyl-3-(trifluoromethyl)phenyl]piperidin-4-ol (2.18 g, yield 32percent) was obtained from 3-iodo-2-methylbenzotrifluoride (6.28 g). 1H-NMR(400MHz,DMSO-d6)delta(ppm) : 1.76-1.91(4H,m), 2.69-2.78(2H,m), 2.71(3H,s), 2.94-3.04(2H,m), 4.91(1H,s), 7.34(1H,t,J=7.8Hz), 7.57(1H,d,J=7.8Hz), 7.70(1H,d,J=7.8Hz).
 

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