6-(TRIFLUOROMETHYL)PYRIDINE-3-METHANOL synthesis

Yield:386704-04-7 92%

Reaction Conditions:

with dimethylsulfide borane complex in tetrahydrofuran at 0 - 20; for 18.5 h;Inert atmosphere;

Steps:

2

The bottom of a room temperature and a nitrogen atmosphere, 6-(trifluoromethyl)-3-pyridinecarboxylic acid (504 mg) 2.64 It cooled at 0 degree C and the dimethylsulfide borane complex (401 mg, 5.27 mmol) was added to the THF solution (8 ml) of mmol, and to the room temperature, the temperature rise was carried out and it agitated for 18.5 hours. Then, it concentrated in vacuum by cooling at 0 degree C and adding methanol. Then, it heated at reflux at 60 degrees C, concentrated in vacuum by having added 1% chloride / methanol and having added triethylamine after cooling at 0 degree C, and obtained the rough product. [6-(trifluoromethyl) pyridin-3-yl] methanol was obtained by refining the obtained rough product with silica gel column chromatography (hexane: ethyl acetate =1:1). Yield 369 mg, 92% of yield, a yellow liquid.

References:

JP2017/178911,2017,A Location in patent:Paragraph 0132; 0133