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
To a solution of compound 46a (90.0 mg, 0.205 mmol) in DCM (2 mL) was added a solution of methanesulfonic acid as a 1 M DCM solution (0.205 mL, 0.205 mmol). The reaction mixture was stirred at rt for 30 min and concentrated under reduced pressure to obtain the title compound 129. 1H-NMR (400 MHz, CDCl3) δ (ppm): 2.81 (s, 6H), 3.92-4.03 (m, 4H), 4.57 (br. s., 4H), 5.78 (s, 2H), 7.18 (d, J=9.0 Hz, 1H), 7.47-7.56 (m, 1H), 7.70 (s, 1H), 7.75 (td, J=7.8, 1.3 Hz, 1H), 7.83 (d, J=7.8 Hz, 1H), 7.94 (d, J=8.3 Hz, 1H), 8.01 (dd, J=8.1, 5.6 Hz, 1H), 8.18 (s, 1H), 8.27 (d, J=8.8 Hz, 1H), 8.54-8.62 (m, 1H), 8.90-8.97 (m, 1H), 9.16 (d, J=1.7 Hz, 1H). Mass Spectrum (LCMS, ESI pos.) Calcd. for C25H22N6O2: 439.1 (M+H). Found 439.1.
WORKUP
后处理
- concentrationconcentrated under reduced pressure