反应详情

After tert-butyl 3-(trifluoromethyl)-3-hydroxypiperidine-1-carboxylate (709 mg, 2.63 mmol) was dissolved in THF (10 ml), followed by addition of HCl (2.0M solution in diethyl ether, 30 ml), and then the resulting mixture was stirred at room temperature for 2 hours. The resulting reaction liquid was concentrated under reduced pressure and dried under vacuum, and then the residue thus obtained was dissolved in acetonitrile (30 ml). 6-Bromopicolinic acid (638 mg, 3.16 mmol) was added thereto, and cooled to 0° C. N,N-Diisopropylethylamine (1.1 ml, 6.58 mmol) and HBTU (1.2 g, 3.16 mmol) were sequentially added thereto, and then the resulting mixture was stirred at room temperature under nitrogen stream for 20 hours. The resulting reaction liquid was concentrated under reduced pressure, followed by addition of MC (50 ml), and then washed with distilled water. The organic layer was dried over anhydrous magnesium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (3% MeOH/MC), to obtain 800 mg of white solid (86%).

1. customThe resulting reaction liquid
2. concentrationwas concentrated under reduced pressure
3. customdried under vacuum
4. customthe residue thus obtained
5. temperaturecooled to 0° C
6. stirringthe resulting mixture was stirred at room temperature under nitrogen stream for 20 hours
7. customThe resulting reaction liquid
8. concentrationwas concentrated under reduced pressure
9. additionfollowed by addition of MC (50 ml)
10. washwashed with distilled water
11. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
12. filtrationfollowed by filtration and concentration
13. customthe residue thus obtained