HRID131173

反应详情

EQUATION

反应方程式

HRID 131173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

PtO2 (528 mg, 2.33 mmol) was added to a dry flask. Ethanol (70 mL), tetrahydrofuran (70 mL), and hydrogen chloride (7.6 mL, 2N) were added after the flask was flushed with argon. Quinolin-7-ol (1000 mg, 6.89 mmol) was added into the flask under argon atmosphere. The solution was degassed and flashed with argon. Hydrogen gas was introduced to the flask by a balloon. The mixture was stirred at H2 atmosphere at room temperature overnight. The mixture was filtered and the filtrate was concentrated. The resulting residue was purified by MPLC (biotage) to afford 730 mg (71%) of the title compound. 1H-NMR (CDCl3) δ 6.77 (d, J=7.6 Hz, 1H), 6.10 (dd, J=8.0 Hz, 2.8 Hz, 1H), 5.95 (d, J=2.4Hz, 1H), 3.24 (t, J=5.9 Hz, 2H), 2.66 (t, J=5.9Hz, 2H), 2.44 (m, 2H); Rf=0.74, 50% ethyl acetate-hexane.

WORKUP

后处理

  1. customwas flushed with argon
  2. customThe solution was degassed
  3. additionHydrogen gas was introduced to the flask by a balloon
  4. filtrationThe mixture was filtered
  5. concentrationthe filtrate was concentrated
  6. customThe resulting residue was purified by MPLC (biotage)