反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A suspension of methyl 2-(2-((2-(4-(1-(tert-butoxycarbonylamino)ethyl)phenylamino)-5-(trifluoromethyl)pyrimidin-4-yl)ethynyl)phenyl)acetate (A64) (353 mg, 0.637 mmol) and Pd/C (10%; 250 mg) in EtOAc (13 mL) was stirred under a hydrogen atmosphere at room temperature overnight. The resulting mixture was filtered through a pad of Celite then the filtrate evaporated under reduced pressure to give the title compound A65 as an off white solid (320 mg, 90%); 1H NMR (300 MHz, CDCl3) δ 8.56 (s, 1H), 7.61 (d, J=8.64 Hz, 2H), 7.52 (s, 1H), 7.28 (m, 5H), 4.81 (m. s, 2H), 3.77 (s, 2H), 3.70 (s, 3H), 3.13 (m, 4H), 1.66 (m, 1H, peak obscured), 1.48 (d, J=6.54 Hz, 3H), 1.45 (s, 9H). LCMS-B: rt 9.07 min; m/z 559.5 [M+H]+.
WORKUP
后处理
- filtrationThe resulting mixture was filtered through a pad of Celite
- customthe filtrate evaporated under reduced pressure