反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A round bottom flask was charged with (2R)-3-(tert-butyldimethylsilyloxy)-2-(5-(2-(3,4-dichlorophenyl)propanamido)-1-oxoisoquinolin-2(1H)-yl)-N-methylpropanamide (60 mg, 0.0001 mol), tetrahydrofuran (3 mL, 0.04 mol) and tetra-n-butylammonium fluoride (0.037 mL, 0.00012 mol) and the reaction stirred at room temperature for 30 minutes during which time the reaction was complete. The solvent was removed under reduced pressure and the residue purified by preparative HPLC (reverse phase) to yield the product as a white solid. MS m/z=463.3 (M+H). 1H NMR (400 MHz; DMSO-d6) δ 10.02 (s, 1H), 8.12 (m, 1H), 8.06 (d, J=8.26 Hz, 1H), 7.74 (t, J=7.29 Hz, 1H), 7.68 (d, J=1.82 Hz, 1H), 7.64 (d, J=8.43 Hz, 1H), 7.51 (dd, J=7.97&3.17 Hz, 1H), 7.46-7.42 (m, 2H), 6.37 (dd, J=5.04&2.04 Hz, 1H), 5.47 (t, J=6.94 Hz, 1H), 5.15-5.13 (m, 1H), 4.05 (q, J=7.24 Hz, 1H), 3.95-3.92 (m, 2H), 2.57 (d, J=4.25 Hz, 3H), 1.47 (d, J=7.22 Hz, 3H).
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- customthe residue purified by preparative HPLC (reverse phase)