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[ CAS No. 936247-35-7 ]

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2D
Chemical Structure| 936247-35-7
Chemical Structure| 936247-35-7
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Product Details of [ 936247-35-7 ]

CAS No. :936247-35-7MDL No. :MFCD18259798
Formula : C5H3ClN2O3 Boiling Point : -
Linear Structure Formula :-InChI Key :N/A
M.W :174.54Pubchem ID :18765698
Synonyms :

Computed Properties of [ 936247-35-7 ]

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

Safety of [ 936247-35-7 ]

Signal Word:WarningClass:N/A
Precautionary Statements:P305+P351+P338UN#:N/A
Hazard Statements:H302-H315-H319Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 936247-35-7 ]

  • Upstream synthesis route of [ 936247-35-7 ]
  • Downstream synthetic route of [ 936247-35-7 ]

[ 936247-35-7 ] Synthesis Path-Upstream   1~1

  • 1
  • [ 74115-12-1 ]
  • [ 936247-35-7 ]
YieldReaction ConditionsOperation in experiment
82% at 20℃; Example 15A
5-Chloro-2-nitropyridin-3-ol
With ice cooling, 30 g of 5-chloropyridin-3-ol (232 mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulphuric acid, and, at 0° C., 24 ml of concentrated nitric acid were added slowly.
The reaction was warmed to RT and stirred overnight.
The mixture was stirred into an ice/water mixture and stirred for another 30 min.
The solid was filtered off, washed with cold water and air-dried.
This gave 33 g (82percent of theory) of the title compound, which were used without further purification for the next reaction.
LC-MS (Method 1): Rt=0.60 min
MS (ESneg): m/z=172.9/174.9 (M-H)-
1H NMR (400 MHz, DMSO-d6): δ=7.71 (d, 1H); 8.10 (d, 1H); 12.14 (br. 1H).
82% at 0 - 20℃; Example 7A 5-Chloro-2-nitropyridin-3-ol With ice cooling, 30 g of 5-chloropyridin-3-ol (232 mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulphuric acid, and, at 0° C., 24 ml of concentrated nitric acid were added slowly. The reaction was warmed to RT and stirred overnight. The reaction mixture was stirred into an ice/water mixture and it was stirred for another 30 min. The solid was filtered off, washed with cold water and air-dried. This gave 33 g (82percent of theory) of the title compound, which were used without further purification for the next reaction. LC-MS (Method 2): Rt=0.60 min MS (ESneg): m/z=172.9/174.9 (M-H)- 1H NMR (400 MHz, DMSO-d6): δ=7.71 (d, 1H); 8.10 (d, 1H); 12.14 (br. 1H).
82% at 0 - 20℃; Example 12A
5-Chloro-2-nitropyridin-3-ol
With ice cooling, 30 g of 5-chloropyridin-3-ol (232 mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulphuric acid, and, at 0° C., 24 ml of concentrated nitric acid were added slowly.
The reaction was warmed to RT, stirred overnight and then stirred into an ice/water mixture and stirred for another 30 min.
The solid was filtered off, washed with cold water and air-dried.
This gave 33 g (82percent of theory) of the title compound, which were used without further purification for the next reaction.
LC-MS (Method 2): Rt=0.60 min
MS (ESneg): m/z=172.9/174.9 (M-H)-
1H NMR (400 MHz, DMSO-d6): δ=7.71 (d, 1H); 8.10 (d, 1H); 12.14 (br. 1H).
82% at 0 - 20℃; With ice cooling, 30 g of 5-chloropyridin-3-ol (232 mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulphuric acid, and 24 ml of concentrated nitric acid were added slowly at 0° C.
The mixture was warmed to RT, stirred overnight and then stirred into an ice/water mixture and stirred for another 30 min.
The solid was filtered off, washed with cold water and air-dried.
This gave 33 g (82percent of theory) of the title compound which was used without further purification for the next reaction.
LC-MS (Method 1): Rt=0.60 min
MS (ESneg): m/z=172.9/174.9 (M-H)-
1H-NMR (400 MHz, DMSO-d6): δ=7.71 (d, 1H), 8.10 (d, 1H), 12.14 (br. 1H).
82% at 0 - 20℃; With ice cooling, 30 g of 5-chloropyridin-3-ol (232 mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulphuric acid, and 24 ml of concentrated nitric acid were added slowly at 00 C. The reaction was warmed to RT, stirred overnight and then stirred into an ice/water mixture and stirred for another 30 mm. The solid was filtered off, washed with cold water and air-dried. This gave 33 g (82percent of theory) of the title compound which was used without further purification for the next reaction.10524] LC-MS (Method 1): R=0.60 mm10525] MS (ESneg): mlz=172.9/174.9 (M—H)10526] ‘H-NMR (400 MHz, DMSO-d5): ö=7.71 (d, 1H);8.10 (d, 1H); 12.14 (bt 1H).
82% at 0 - 20℃; With ice cooling, 30 g of 5-chloropyridin-3-ol (232 mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulphuric acid, and 24 ml of concentrated nitric acid were added slowly at 0° C.
The reaction was warmed to RT, stirred overnight and then stirred into an ice/water mixture and stirred for another 30 min.
The solid was filtered off, washed with cold water and air-dried.
This gave 33 g (82percent of theory) of the title compound which was used without further purification for the next reaction.
LC-MS (Method 2): Rt=0.60 min
MS (ESneg): m/z=172.9/174.9 (M-H)-
1H-NMR (400 MHz, DMSO-d6): δ=7.71 (d, 1H); 8.10 (d, 1H); 12.14 (br. 1H).
82% at 0 - 20℃; With ice cooling, 30 g of 5-chloropyridin-3-ol (232 mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulfuric acid, and 24 ml of concentrated nitric acid were added slowly at 0° C.
The reaction was warmed to RT and stirred overnight.
The mixture was stirred into an ice/water mixture and stirred for 30 min.
The solid was filtered off, washed with cold water and air-dried.
This gave 33 g (82percent of theory) of the title compound which was used without further purification for the next reaction.
LC-MS (Method 1): Rt=0.60 min
MS (ESneg): m/z=172.9/174.9 (M-H)-
1H-NMR (400 Mhz, DMSO-d6): δ=7.71 (d, 1H); 8.10 (d, 1H); 12.14 (br. 1H).
82% at 0 - 20℃; With ice cooling, 30 g of 5-chloropyridin-3-ol (232mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulphuric acid, and 24 ml of concentrated nitric acid were added slowly at 0° C. The reaction was warmed to RT and stirred overnight. The mixture was stirred into an ice/water mixture and stirred for 30 mm. The crystals were filtered off, washed with cold water and air-dried. This gave 33 g (82percent of theory) of the title compound which was used without thrther purification for the next reaction.10372] LC-MS (Method 2): R=0.60 mm10373] MS (ESneg): mlz=172.9/174.9 (M—H)j0374] ‘H-NMR (400 MHz, DMSO-d5): ö=7.71 (d, 1H); 8.10 (d, 1H); 12.14 (bt 1H).
74% With sulfuric acid; nitric acid In water at 5 - 20℃; for 3 - 144 h; 5-Chloro-3-pyridinol (15.3 mmol) is dissolved in concentrated H2SO4 (15 ml). At 5 0C concentrated nitric acid (0.9 ml) is added. The reaction mixture is allowed to warm to room temperature over 6 days. The reaction solution is pored onto ice (50 ml) and diluted with water (200 ml). The precipitate is filtered, washed with water and dried at 40 0C in vacuo. 5-Chloro-2-nitro-pyridine-3-ol is obtained as yellow powder; mp. 97°; LC- MS (method B): 1.35 min, 175.1 (M+H+).; 5-Chloro-3-pyridinol (382 mmol) is dissolved in concentrated H2SO4 (375 ml). At 5 0C concentrated nitric acid (25 ml) is added. The reaction is allowed to warm to room temperature over 3 hours. The reaction solution is pored onto ice water (5000 ml). The precipitate is filtered, washed with water and dried over night at 40 0C in vacuo. 5- Chloro-2-nitro-pyridine-3-ol is obtained as yellow powder in a yield of 74 percent. Mp.: 97 0C; LC-MS (Method B): 1.35 min, 175.1 (MH+).
67% at 5 - 20℃; for 3 h; 5-chloropyridin-3-ol(2.00 g, 15.4 mmol) was dissolved in concentrated H2SO4(15 mL) at 5 °C. Concentrated nitric acid (1.0 mL) was then added. The reactionwas allowed to warm to room temperature over 3 hrs. The reaction solution waspoured onto ice water (25 mL). The resultant precipitate was filtered, washedwith water and dried overnight at 40 °C in vacuo to afford was obtained as ayellow powder, (1.80g, 67percent); H NMR (400 MHz, CDCI3) δ7.68 (d, 1H), 8.15 (d, 1H), 10.29 (s, 1H).
33 g at 0 - 20℃; Example 7A
5-Chloro-2-nitropyridin-3-ol
With ice cooling, 30 g of 5-chloropyridin-3-ol (232 mmol, 1 equivalent) were dissolved in 228 ml of concentrated sulphuric acid, and 24 ml of concentrated nitric acid were added slowly at 0° C.
The reaction was warmed to RT, stirred overnight and then stirred into an ice/water mixture and stirred for another 30 min.
The solid was filtered off, washed with cold water and air-dried.
This gave 33 g (82percent of theory) of the title compound which was used without further purification for the next reaction.
LC-MS (Method 1): Rt=0.60 min
MS (ESneg): m/z=172.9/174.9 (M-H)-
1H-NMR (400 MHz, DMSO-d6): δ=7.71 (d, 1H); 8.10 (d, 1H); 12.14 (br. 1H).

Reference: [1] Patent: US2014/128386, 2014, A1, . Location in patent: Paragraph 1052; 1053; 1054; 1056
[2] Patent: US2014/128425, 2014, A1, . Location in patent: Paragraph 0393-0397
[3] Patent: US2014/128372, 2014, A1, . Location in patent: Paragraph 0414; 0415; 0416; 0417; 0418
[4] Patent: US2016/122341, 2016, A1, . Location in patent: Paragraph 0545; 0546; 0547; 0548; 0549
[5] Patent: US2016/347770, 2016, A1, . Location in patent: Paragraph 0522; 0523; 0524; 0525; 0526
[6] Patent: US2017/57958, 2017, A1, . Location in patent: Paragraph 0197-0201
[7] Patent: US2017/304278, 2017, A1, . Location in patent: Paragraph 0696; 0697; 0698; 0699; 0700
[8] Patent: US2016/362408, 2016, A1, . Location in patent: Paragraph 0370; 0371; 0372; 0373; 374
[9] Patent: WO2009/46784, 2009, A1, . Location in patent: Page/Page column 60; 71
[10] Patent: WO2014/184234, 2014, A1, . Location in patent: Page/Page column 69
[11] Patent: US2017/50961, 2017, A1, . Location in patent: Paragraph 0929; 0930; 0931; 0932; 0933
[12] Patent: US2017/57954, 2017, A1, . Location in patent: Paragraph 0542; 0543; 0544l 0545; 0546
[13] Patent: US2017/217954, 2017, A1,
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