HRID718653
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
A solution of compound 52e (45 mg, 0.070 mmol) in TFA:DCM (1:3 v/v, 5 mL) was stirred overnight at rt. The resulting mixture was concentrated under reduced pressure and the residue obtained was treated with Et2O (10 mL). The solids formed were collected by filtration and washed with Et2O (2×20 mL). The title compound 59 was obtained as a yellow solid. 1H-NMR (300 MHz, DMSO-d6) δ (ppm): 8.92 (d, J=8.4 Hz, 1H), 8.87 (s, 1H), 8.25 (d, J=8.4 Hz, 1H), 8.06-8.03 (m, 3H), 7.94-7.85 (m, 2H), 7.72 (d, J=8.4 Hz, 2H), 7.64 (d, J=8.4 Hz, 2H), 6.30 (d, J=5.7 Hz, 1H), 3.56-3.43 (m, 12H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C29H26N8O2: 519.2 (M+H). Found: 519.1.
WORKUP
后处理
- concentrationThe resulting mixture was concentrated under reduced pressure
- customthe residue obtained
- customThe solids formed
- filtrationwere collected by filtration
- washwashed with Et2O (2×20 mL)