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Chemical Structure| 329927-16-4 Chemical Structure| 329927-16-4

Structure of 329927-16-4

Chemical Structure| 329927-16-4

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Product Details of [ 329927-16-4 ]

CAS No. :329927-16-4
Formula : C7H7FIN
M.W : 251.04
SMILES Code : NC1=CC=C(I)C(F)=C1C
MDL No. :MFCD21364950

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Application In Synthesis of [ 329927-16-4 ]

* 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 [ 329927-16-4 ]

[ 329927-16-4 ] Synthesis Path-Downstream   1~3

  • 1
  • [ 443-86-7 ]
  • [ 329927-16-4 ]
YieldReaction ConditionsOperation in experiment
95% a) Compound 5.2 To a solution of aniline 5.1 (5.20 g, 41.6 mmol) in acetic acid (30 mL) was added Kl (8.46 g, 51 mmol), NaBO3.4H2O (7.28 g, 47 mmol) and (NH4)2MoO4 (7.9 g, 40 mmol). After 30 min the reaction was poured into a mixture of aqueous saturated NaHCO3 solution (50 mL) and aqueous 10percent Na2S2O3 solution (10 mL). The aqueous layer was extracted with Et2O and the combined organic phases were washed with brine, dried (MgSO4) filtered and concentrated under reduced pressure to give compound 5.2 (9.96 g, 95percent yield) as a beige solid.
75% With sodium perborate tetrahydrate; acetic acid; potassium iodide; In water; at 0 - 20℃; for 1.5h; To a stirred solution of 3-fluoro- 2-methylaniline (10.0 g, 0.080 mmol) in acetic acid/water (1:1 ratio, 100 mL) was added NaBO3.4H20 (12.3 g, 0.080 mmol). At 0°C, a solution of KI (13.3 g, 0.080 mmol) in 100 mL water was added dropwise over 30 mm. After being stirred at ft for lh, the mixture was diluted with water, filtered, and air dried to afford 1-1 (15.0 g, 75percent) as a brown solid. LCMS:251.86 [M+H]
With Iodine monochloride; In acetic acid; at 70℃; for 2h; Iodine monochloride (0.5 ml) was added to a solution of <strong>[443-86-7]3-fluoro-2-methylaniline</strong> (1.25 g) in glacial acetic acid (15 ml). The mixture was stirred for two hours at 70° C. The mixture was allowed to cool to ambient temperature and saturated sodium sulphite solution (50 ml) was added. The solution was extracted with EtOAc (2.x.100 ml), and the extracts were combined, washed with saturated sodium bicarbonate solution (100 ml) and dried. The volatile material was removed by evaporation and the residue was purified by chromatography on silica gel, eluted with 0-10percent EtOAc in hexane to give the title compound (1.53 g) as a solid. NMR: 1.98 (s, 3H), 5.32 (s, 2H), 6.30 (d, 1H), 7.20 (t, 1H); m/z: 250.
  • 2
  • [ 329927-16-4 ]
  • [ 124-38-9 ]
  • [ 194804-84-7 ]
  • [ 443-86-7 ]
  • 3
  • [ 443-86-7 ]
  • [ 329927-16-4 ]
  • [ 1364740-03-3 ]
  • [ 1364740-08-8 ]
 

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