preparation method of 1h-pyrazole-5-potassium trifluoroborate_industrial additives

background and overview of the preparation method of 1h-pyrazole-5-potassium trifluoroborate

1h-pyrazole-5-potassium trifluoroborate can be used as a pharmaceutical synthesis intermediate. if 1h-pyrazole-5-trifluoroborate potassium is inhaled, move the patient to fresh air; if skin contact occurs, take off contaminated clothing, rinse the skin thoroughly with soap and water, and seek medical attention if you feel uncomfortable.

preparation method of potassium 1h-pyrazole-5-trifluoroborate

1h-pyrazole-5-potassium trifluoroborate can be used as a pharmaceutical synthesis intermediate, if the following reaction occurs:

a mixture of 1h-pyrazole-5-boronic acid (150 mg, 1.34 mmol) and potassium hydrofluoride (262 mg, 3.35 mmol) in 1:3 methanol/water (2 ml) was stirred at room temperature overnight. the mixture was transferred to a vial, the vial was sealed and the mixture was heated to 100°c in an oil bath for 2 hours to produce a solution. the solution was cooled and concentrated. the solid was slurried in hot acetone, filtered and the filtrate concentrated to provide potassium 1h-pyrazole-5-trifluoroborate (234 mg, 100%). 2-amino-6-bromo-8-((trans)-4-hydroxycyclohexyl)-4-methylpyrido[2,3-d]pyrimidin-7(8h)-one (100 mg, 0.283 mmol) a mixture of potassium 1h-pyrazole-5-trifluoroborate (98.5 mg, 0.566 mmol) and triethylamine (197 μl, 1.42 mmol) in ethanol (3.0 ml) was bubbled with argon. pdcl2 (dppf) 1:1 w/ch2cl lanthanum 2 carbonate was added, the vial was sealed and the mixture was sparged with argon again, then heated in the microwave at 100°c for 30 minutes and then at 150°c for 60 minutes. the reaction mixture was concentrated and purified by flash chromatography eluting with 1:1 ethyl acetate:chloroform/7n ammonia in methanol (0.5-7%). fractions containing the desired product were combined and concentrated and the solid was recrystallized from methanol/chloroform to provide 2-amino-8-((trans)-4-hydroxycyclohexyl)-4-methyl-6-(1h- sodium pyrazol-3-yl)pyrido[2 carbonate, 3-d]pyrimidin-7(8h)-one (32 mg, 33%).

1h nmr (mhz, dmso-d 6 ) δppm 1.24-1.35 (m, 2h) 1.44-1.55 (m, 2 h) 1.90-1.99 (m, 2h) 2.56 (s, 3h) 2.73-2.84 (m , 2h) 3.50-3.62 (m, 1h) 4.62 (d, j = 4.04hz, 1h) 5.12-5.74 (m, 1h) 6.93 (s, 1h) 7.14-7.26 (m, 2h) 7.62 (m, 1h) 8.34(s,1h)12.97(m,1h)