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Chemical Structure| 22280-56-4 Chemical Structure| 22280-56-4
Chemical Structure| 22280-56-4

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CAS No.: 22280-56-4

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Synonyms: 2-Chloro-5-nitro-3-picoline

4.5 *For Research Use Only !

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Product Details of 2-Chloro-3-methyl-5-nitropyridine

CAS No. :22280-56-4
Formula : C6H5ClN2O2
M.W : 172.57
SMILES Code : C1=C(C=NC(=C1C)Cl)[N+](=O)[O-]
Synonyms :
2-Chloro-5-nitro-3-picoline
MDL No. :MFCD00173686
InChI Key :OSIOIGXJUZTWRI-UHFFFAOYSA-N
Pubchem ID :89648

Safety of 2-Chloro-3-methyl-5-nitropyridine

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H301-H315-H318-H335
Precautionary Statements:P261-P280-P301+P310-P305+P351+P338
Class:8(6.1)
UN#:2923
Packing Group:Ⅲ

Application In Synthesis of 2-Chloro-3-methyl-5-nitropyridine

* 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.

  • Upstream synthesis route of [ 22280-56-4 ]
  • Downstream synthetic route of [ 22280-56-4 ]

[ 22280-56-4 ] Synthesis Path-Upstream   1~4

  • 1
  • [ 22280-56-4 ]
  • [ 38186-82-2 ]
YieldReaction ConditionsOperation in experiment
97% With iron; acetic acid In water for 3 h; Iron (Fe) powder (9.75 g, 0.174 mol, Sigma-Aldrich) was added in portions over a period of 2h to a stirred solution of 2-chloro-3-methyl-5-nitropyridine (10 g, 0.058 mol, Combi-blocks) in acetic acid/water (29 mL: 88 mL). After 3h, the reaction mixture was filtered through celite and the filter cake was washed with ethyl acetate. The organic layer was separated and the aqueous layer was extracted with EtOAc. The combined organic layers were washed with aqueous sodium bicarbonate, brine and dried over Na2S04. The solvent was removed under reduced pressure to yield 6-chloro-5-methylpyridine-3-amine as a brown solid (8.0g; 97percent). MS m/z = 142.03 [M+H]+.1H-NMR (300MHZ, DMSO-d6): 7.54 (d, J=30 Hz, 1H), 6.91-6.90 (dd, J = 0.6 Hz & 2.7 Hz, 1H), 5.39 (s, 2H), 2.17 (s, 3H)
97% With iron; acetic acid In water for 5 h; Iron powder (9.75 g, 0.17 mol) was added in portions over a period of 2 h to a stirred solution of 2-chloro-3-methyl-5-nitropyridine (10 g, 58.00 mmol, Combi-blocks) in HOAc/water (29 mL : 88 mL). After 3 h, the reaction mixture was filtered through Celite? filter aid and the filter cake was washed with EtOAc. The organic layer was separated and the aqueous layer was extracted with EtOAc. The combined organic layers were washed with aqueous sodium bicarbonate, brine and dried over Na2SO4. The solvent was removed under reduced pressure to yield 6-chloro-5- methylpyridine-3-amine as a brown solid (269A, 8.00 g; 97percent). MS m/z = 142.03 [M+H]+. 1H-NMR (300MHz, DMSO-d6): 7.54 (d, J=30 Hz, 1 H), 6.91 -6.90 (dd, J = 0.6 Hz & 2.7 Hz, 1 H), 5.39 (s, 2H), 2.17 (s, 3H)
42% With water; iron; ammonium chloride In methanol at 20 - 50℃; for 3.08333 h; Heating / reflux Reference Example 33 6-chloro-5-methylpyridine-3-amine; Reduced iron (793 mg) was added to an aqueous solution (25 mL) of ammonium chloride (1.27 g), and the mixture was stirred at room temperature for 5 min. A solution (10 mL) of 2-chloro-3-methyl-5-nitropyridine (816 mg) in methanol was added dropwise over 10 min. The reaction mixture was stirred at 40° C. for 20 min and at 50° C. for 1.5 hr and further refluxed for 1 hr. The reaction mixture was filtered through celite, and celite was washed with methanol. Methanol was mostly removed by concentration under reduced pressure, and saturated aqueous sodium hydrogencarbonate solution was added. The mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=19:1-->7:3) to give the title compound as a solid (yield 280 mg, 42percent). 1H-NMR (CDCl3) δ: 3.62 (2H, br), 6.88-6.89 (1H, m), 7.70-7.71 (1H, m).
42% With iron; ammonium chloride In methanol at 40℃; for 2.83333 h; Heating Reference Example 136
6-Chloro-5-methylpyridine-3-amine
Reduced iron (793 mg) was added to an aqueous solution (25 mL) of ammonium chloride (1.27 g), and the mixture was stirred at room temperature for 5 min.
A solution (10 mL) of 2-chloro-3-methyl-5-nitropyridine (816 mg) in methanol was added dropwise over 10 min.
The reaction mixture was stirred at 40°C for 20 min and at 50°C for 1.5 hr and further refluxed under heating for 1 hr.
The reaction mixture was filtered through celite, and celite was washed with methanol.
Methanol was mostly removed by concentrated under reduced pressure, and saturated aqueous sodium hydrogencarbonate solution was added.
The mixture was extracted with ethyl acetate.
The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure.
The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=19:1→7:3) to give the title compound as a solid (yield 280 mg, 42percent).
1H-NMR (CDCl3)δ: 2.29 (3H, s), 3.62 (2H, br), 6.88-6.89 (1H, m), 7.70-7.71 (1H, m).

References: [1] Patent: WO2014/138484, 2014, A1, . Location in patent: Page/Page column 156.
[2] Patent: WO2016/22724, 2016, A1, . Location in patent: Page/Page column 296.
[3] Journal of Organic Chemistry, 2011, vol. 76, # 23, p. 9841 - 9844.
[4] Synthetic Communications, 2006, vol. 36, # 9, p. 1235 - 1245.
[5] Organic Letters, 2016, vol. 18, # 11, p. 2774 - 2776.
[6] Chemistry of Heterocyclic Compounds, 1996, vol. 32, # 10, p. 1173 - 1177.
[7] Patent: US2007/60623, 2007, A1, . Location in patent: Page/Page column 24.
[8] Patent: WO2006/36024, 2006, A1, . Location in patent: Page/Page column 162.
[9] Patent: EP2336107, 2015, B1, . Location in patent: Paragraph 0310.
[10] Patent: WO2007/65662, 2007, A2, . Location in patent: Page/Page column 44.
[11] Patent: US2014/249104, 2014, A1, . Location in patent: Page/Page column.
[12] Patent: WO2005/123668, 2005, A1, . Location in patent: Page/Page column 46-47.
  • 2
  • [ 22280-56-4 ]
  • [ 7732-18-5 ]
  • [ 7439-89-6 ]
  • [ 38186-82-2 ]
YieldReaction ConditionsOperation in experiment
89% With acetic acid In ethyl acetate 19a.
5-Amino-2-chloro-3-methylpyridine
2-Chloro-3-methyl-5-nitropyridine (15 g, 86.9 mmol; from Maybridge Chemical Co.) was dissolved in a solution of H2 O/AcOH (5:1, 60 mL).
Iron powder was added to the reaction mixture while maintaining the temperature below 40° C., and the mixture was stirred for 5 hours.
The mixture was filtered through celite and the aqueous filtrate was extracted with EtOAc (4*).
The filter cake was washed with EtOAc, and the EtOAc solutions were combined, dried (MgSO4), concentrated and chromatographed (silica gel; CHCl3 /MeOH, 98:2) to afford an orange solid (2.3 g, 89percent): 1 H NMR (CD3 OD, 300 MHz) δ2.25 (s, 3H), 7.01 (d, J=2.0 Hz, 1H), 7.58 (d, J=2.0 Hz, 1H); MS (CI/NH3) m/z: 243/245 (M+H)+.
References: [1] Patent: US5733912, 1998, A, .
  • 3
  • [ 22280-56-4 ]
  • [ 7732-18-5 ]
  • [ 7439-89-6 ]
  • [ 54232-03-0 ]
  • [ 38186-82-2 ]
References: [1] Patent: US6133253, 2000, A, .
  • 4
  • [ 22280-56-4 ]
  • [ 144-55-8 ]
  • [ 38186-82-2 ]
References: [1] Patent: EP1803709, 2007, A1, .
 

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