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5-Trifluoromethyl-pyridine-3-boronic acid

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5-Trifluoromethyl-pyridine-3-boronic acid Basic information
Product Name:5-Trifluoromethyl-pyridine-3-boronic acid
Synonyms:5-Trifluoromethyl-pyridine-3-boronic acid;3-trifluoromethyl-5-pyridyl boronic acid;(5-Trifluoromethylpyridin-3-yl)boronic acid, 95%;5-TRIFLUOROMETHYL-PYRIDINE-3-BORONIC ACI;BP 33117 5-TRIFLUOROMETHYL-PYRIDINE-3-BORONIC ACID;3-Borono-5-(trifluoromethyl)pyridine;5-TrifluoroMethyl-3-pyridineboric acid;[5-(Trifluoromethyl)-3-pyridyl]boronic acid
CAS:947533-51-9
MF:C6H5BF3NO2
MW:190.92
EINECS:
Product Categories:
Mol File:947533-51-9.mol
5-Trifluoromethyl-pyridine-3-boronic acid Structure
5-Trifluoromethyl-pyridine-3-boronic acid Chemical Properties
Melting point 300.8 °C (decomp)
Boiling point 299.9±50.0 °C(Predicted)
density 1.44±0.1 g/cm3(Predicted)
storage temp. under inert gas (nitrogen or Argon) at 2-8°C
form Crystalline Powder
pka5.90±0.10(Predicted)
color White to yellow
InChIInChI=1S/C6H5BF3NO2/c8-6(9,10)4-1-5(7(12)13)3-11-2-4/h1-3,12-13H
InChIKeySFBQNNGMEKUJAN-UHFFFAOYSA-N
SMILESB(C1=CC(C(F)(F)F)=CN=C1)(O)O
Safety Information
HS Code 29333999
MSDS Information
5-Trifluoromethyl-pyridine-3-boronic acid Usage And Synthesis
Synthesis
Triisopropyl borate

5419-55-6

3-Bromo-5-(trifluoromethyl)pyridine

436799-33-6

5-Trifluoromethyl-pyridine-3-boronic acid

947533-51-9

Under nitrogen protection, 3-bromo-5-(trifluoromethyl)pyridine (2.5 g, 11.06 mmol) and triisopropyl borate (3.06 mL, 13.27 mmol) were dissolved in anhydrous tetrahydrofuran (20 mL) and cooled to -78 °C. A hexane solution of n-butyllithium (2.5 M, 4.9 mL, 12.17 mmol) was slowly added dropwise, keeping the reaction mixture stirred at -78 °C for 3 hours. Subsequently, the reaction mixture was slowly warmed to -10 °C. The reaction was quenched by addition of water (20 mL) and the tetrahydrofuran was removed by distillation under reduced pressure. The remaining aqueous phase was diluted with water (40 mL) and washed with ether (2 x 40 mL). The aqueous phase was adjusted to pH 5 with acetic acid and the resulting suspension was extracted with ethyl acetate (80 mL). The organic phase was separated, dried with anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to give 3-(trifluoromethyl)pyridine-5-boronic acid as a brown solid (2.022 g, 96% yield). HPLC/MS analysis: retention time 1.47 min, mass-to-charge ratio 192.1 (M+H+).

References[1] Patent: US2014/135320, 2014, A1. Location in patent: Paragraph 0224; 0225
5-Trifluoromethyl-pyridine-3-boronic acid Preparation Products And Raw materials
Raw materialsn-Butyllithium-->Triisopropyl borate-->Water-->3-Bromo-5-(trifluoromethyl)pyridine-->Hexane-->Tetrahydrofuran
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