HRID718653

反应详情

EQUATION

反应方程式

HRID 718653 的结构方程式

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

  1. concentrationThe resulting mixture was concentrated under reduced pressure
  2. customthe residue obtained
  3. customThe solids formed
  4. filtrationwere collected by filtration
  5. washwashed with Et2O (2×20 mL)