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[ CAS No. 1033202-14-0 ]

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2D
Chemical Structure| 1033202-14-0
Chemical Structure| 1033202-14-0
Structure of 1033202-14-0 *Storage: {[proInfo.prStorage]}

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Product Details of [ 1033202-14-0 ]

CAS No. :1033202-14-0MDL No. :MFCD10699675
Formula : C5H3FN2O3 Boiling Point : 244.4±40.0°C at 760 mmHg
Linear Structure Formula :-InChI Key :N/A
M.W :158.09Pubchem ID :-
Synonyms :

Computed Properties of [ 1033202-14-0 ]

TPSA : - H-Bond Acceptor Count : -
XLogP3 : - H-Bond Donor Count : -
SP3 : - Rotatable Bond Count : -

Safety of [ 1033202-14-0 ]

Signal Word:WarningClass:N/A
Precautionary Statements:P261-P305+P351+P338UN#:N/A
Hazard Statements:H302-H315-H319-H335Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 1033202-14-0 ]

  • Upstream synthesis route of [ 1033202-14-0 ]
  • Downstream synthetic route of [ 1033202-14-0 ]

[ 1033202-14-0 ] Synthesis Path-Upstream   1~1

  • 1
  • [ 1033202-14-0 ]
  • [ 1079179-12-6 ]
YieldReaction ConditionsOperation in experiment
97% at 60℃; for 10 h; To a stirred solution of 3-fluoro-5-nitropyridin-2-ol (1.5 g, 9.48 mmol) in phosphorous oxychloride (15 ml_) was added phosphorous pentachloride (2.96 g, 14.22 mmol) at 60 °C. The reaction mixture was allowed to stir for 10h at the same temperature. The reaction mixture was cooled to ambient temperature and was poured into crushed ice and was extracted with ethyl acetate (3 x 20 mL). The total organic layer was washed with saturated sodium carbonate solution (25 ml_).The washed organic layer was dried over anhydrous magnesium sulfate and was concentrated under reduced pressure to obtain crude compound which was purified by using silica gel column chromatography (100-200 mesh, 5 percent ethyl acetate in hexane) to afford 2-chloro-3-fluoro-5-nitropyridine (1.62 g, 97 percent).
97% at 60℃; for 10 h; To a stirred solution of 3-fluoro-5-nitropyridin-2-ol (1.5 g, 9.48 mmol) in phosphorous oxychloride (15 mL) was added phosphorous pentachloride (2.96 g, 14.22 mmol) at 60 °C. The reaction mixture was allowed to stir for 10 h at the same temperature. The reaction mixture was cooled to room temperature and was poured into crushed ice and was extracted with ethyl acetate (3 x 20 mL). The total organic layer was washed with saturated sodium carbonate solution (25 mL). The washed organic layer was dried over anhydrous magnesium sulphate and was concentrated under reduced pressure to obtain crude compound which was purified by using column chromatography (silica gel: 100-200 mesh, eluent: 5 percent ethyl acetate in n-hexane) to afford 2-chloro-3-fluoro-5-nitropyridine (1.62 g, 97 percent).
97% With phosphorus pentachloride; trichlorophosphate In hexane; ethyl acetate at 60℃; for 10 h; Step 1:
To a stirred solution of 3-fluoro-5-nitropyridin-2-ol (1.5 g, 9.48 mmol) in phosphorous oxychloride (15 mL) was added phosphorous pentachloride (2.96 g, 14.22 mmol) at 60° C.
The reaction mixture was allowed to stir for 10 h at the same temperature.
The reaction mixture was cooled to ambient temperature and was poured into crushed ice and was extracted with ethyl acetate (3*20 mL).
The total organic layer was washed with saturated sodium carbonate solution (25 mL).
The washed organic layer was dried over anhydrous magnesium sulfate and was concentrated under reduced pressure to obtain crude compound which was purified by using silica gel column chromatography (100-200 mesh, 5percent ethyl acetate in hexane) to afford 2-chloro-3-fluoro-5-nitropyridine (1.62 g, 97percent).
97% With phosphorus pentachloride; trichlorophosphate In hexane at 60℃; for 10 h; Step 1
To a stirred solution of 3-fluoro-5-nitropyridin-2-ol (1.5 g, 9.48 mmol) in phosphorous oxychloride (15 mL) was added phosphorous pentachloride (2.96 g, 14.22 mmol) at 60° C.
The reaction mixture was allowed to stir for 10 h at the same temperature.
The reaction mixture was cooled to room temperature and was poured into crushed ice and was extracted with ethyl acetate (3*20 mL).
The total organic layer was washed with saturated sodium carbonate solution (25 mL).
The washed organic layer was dried over anhydrous magnesium sulfate and was concentrated under reduced pressure to obtain crude compound which was purified by using column chromatography (silica gel: 100-200 mesh, eluent: 5percent ethyl acetate in n-hexane) to afford 2-chloro-3-fluoro-5-nitropyridine (1.62 g, 97percent).

Reference: [1] Patent: WO2013/13817, 2013, A1, . Location in patent: Page/Page column 96; 97
[2] Patent: WO2013/13815, 2013, A1, . Location in patent: Page/Page column 131
[3] Patent: US2013/29961, 2013, A1, . Location in patent: Paragraph 0656
[4] Patent: US2013/29962, 2013, A1, . Location in patent: Paragraph 0761
[5] MedChemComm, 2016, vol. 7, # 5, p. 1022 - 1032
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