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[ CAS No. 251300-28-4 ]

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Chemical Structure| 251300-28-4
Chemical Structure| 251300-28-4
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Product Details of [ 251300-28-4 ]

CAS No. :251300-28-4 MDL No. :MFCD03788530
Formula : C7H4BrFO2 Boiling Point : 226.0±35.0°C at 760 mmHg
Linear Structure Formula :- InChI Key :N/A
M.W :219.01 g/mol Pubchem ID :-
Synonyms :

Safety of [ 251300-28-4 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P305+P351+P338 UN#:N/A
Hazard Statements:H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 251300-28-4 ]

  • Upstream synthesis route of [ 251300-28-4 ]
  • Downstream synthetic route of [ 251300-28-4 ]

[ 251300-28-4 ] Synthesis Path-Upstream   1~3

  • 1
  • [ 251300-28-4 ]
  • [ 341-27-5 ]
Reference: [1] Synthesis, 1999, # 11, p. 1878 - 1880
  • 2
  • [ 251300-28-4 ]
  • [ 286836-04-2 ]
Reference: [1] Patent: WO2011/103546, 2011, A1,
  • 3
  • [ 251300-28-4 ]
  • [ 876861-29-9 ]
YieldReaction ConditionsOperation in experiment
98% With dihydrogen peroxide; sodium hydroxide In tetrahydrofuran; water at 0 - 20℃; for 6.5 h; [000236] To a solution of Compound C2 (40 g, 183 mmol) in THF (260 mL) was added dropwise aq. NaOH solution (0.05 N, 720 mL, 37 mmol) at 0 °C, and then 30percent> H202 solution (90 mL). The mixture was stirred for 2 h at rt and followed by the addition of a second portion of 30percent H202 (90 mL). After stirred for 4 h, it was cooled to 0 °C and aq. NaOH solution (2 N, 112 mL) was added until pH10~l 1 was reached, and then the mixture was stirred for 0.5 h and quenched with cone. HC1 at 0 °C to pH2~3. It was extracted with dichloromethane (250 mL x 3) and washed with brine (300 mL x 2), dried over Na2S04, and concentrated to give Compound C3 (37 g, yield 98percent) as a yellow oil. LC-MS (m/z): 205 [M-
92% With sodium hydroxide; water; dihydrogen peroxide In water at 20 - 30℃; for 2.08333 h; To a 1 N aqueous solution of sodium hydroxide (230 mL, 0.23 mol), 5-bromo-3-fluoro-2-hydroxybenzaldehyde (45.0 g, 0.21 mol) was added at room temperature, and a 6percent hydrogen peroxide solution (225 mL) was added dropwise over five minutes at room temperature. After the reaction mixture was stirred at room temperature for two hours, a saturated aqueous solution of sodium thiosulfate (150 mL) was added thereto at room temperature. The mixture was extracted three times with ethyl acetate (450 mL), the organic layer was washed sequentially with a 1 N aqueous solution of hydrochloric acid (150 mL) and saturated saline, dried over anhydrous magnesium sulfate, and filtered through silica gel. The solvent was distilled off from the resultant filtrate under reduced pressure to give 39.0 g of the title compound (yield: 92percent). 1H-NMR (400 MHz, CDCl3) : 6.89 (1H, dd, J = 2,2 Hz), 6.85 (1H, dd, J = 9,2 Hz).
82% With dihydrogen peroxide; sodium hydroxide In tetrahydrofuran; water at 0℃; for 6 h; To a solution of 3-fluoro-2-hydroxybenzaldehyde (5 g, 35.6 mmol) in MeCN (40mL) was added NBS (6.008 g, 36 mmol) and CH3CO2NH4 (270 mg, 3.56 mmol) at RT and the mixture was stirred at RT for 2 h, poured into H20 (30 mL) and extracted with EA (20 mL x 2). The organic layers were dried over anhydrous Na2SO4, filtered, concentrated in vacuo, and the residue purified by silica gel column chromatography (PE/EA = 8/1 to 4/1) to afford 5-bromo- 3-fluoro-2-hydroxybenzaldehyde (6.6 g, 85 percent) as a yellow solid. ‘H NMR (400 MI-Tz, DMSO10 d6) ö 11.24 (s, 1H), 10.22 (s, 1H), 7.84 (dd, J= 10.4 Hz, 2.4 Hz, 1H), 7.59 (dd, J 2.4 Hz, 1.6Hz, 1H). LC-MS: tR= 1.284 mm.
Reference: [1] Patent: WO2015/42397, 2015, A1, . Location in patent: Paragraph 000236
[2] Patent: EP1780192, 2007, A1, . Location in patent: Page/Page column 11
[3] Patent: WO2017/176960, 2017, A1, . Location in patent: Paragraph 00730
[4] Patent: WO2015/65937, 2015, A1, . Location in patent: Paragraph 000213
[5] Patent: WO2016/145153, 2016, A1, . Location in patent: Paragraph 000179
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