反应详情

A solution of (S)-6-(2-hydroxy-2-methylpropyl)-6-phenyl-3-((S)-piperidin-3-yl)-1,3-oxazinan-2-one TFA salt (12 mg, 0.036 mmol), 2,3-difluoropyridine (6 mg, 2equiv), and i-Pr2NEt (30 μL, 5 equiv) in 1:6 MeOH/n-Propanol (2 mL) was heated in the microwave oven for 15 min. at 150° C. After being cooled to rt, the mixture was acidified with 5% aq HCl solution and purified by prep HPLC to afford (S)-3-((S)-1-(3-fluoropyridin-2-yl)piperidin-3-yl)-6-(2-hydroxy-2-methylpropyl)-6-phenyl-1,3-oxazinan-2-one (5.8 mg, 50% yield). LC-MS Method 1 tR=1.51 min, m/z=428(M+1); 1H NMR (CD3OD) 7.92(dd, 1H), 7.51-7.28(m, 6H), 6.88(m, 1H), 4.10(m, 1H), 3.91(m, 2H), 3.06(td, 1H), 2.51(m, 2H), 2.19(s, 2H), 1.24(s, 3H), 0.94(s, 3H).

1. custompurified by prep HPLC