HRID657769

反应详情

EQUATION

反应方程式

HRID 657769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

Methyl quinoline-7-carboxylate (5 g, 0.01 mol) was dissolved in tetrahydrofuran (40 mL) at −20° C. under an atmosphere of nitrogen. 60% REDAL (60:40, Red-Al(R):toluene, 6.53 mL, 0.0201 mol) was added and allowed to stir at −20° C. for 4 hours. After warming to room temperature, the reaction was quenched slowly with water, concentrated under reduced pressure, partitioned between EtOAc and water, and filtered through Celite. The aqueous phase was extracted with EtOAc. The combined organic layers were dried with MgSO4, and concentrated under reduced pressure. The residue was purified by silica gel column to afford the title compound.

WORKUP

后处理

  1. temperatureAfter warming to room temperature
  2. customthe reaction was quenched slowly with water
  3. concentrationconcentrated under reduced pressure
  4. custompartitioned between EtOAc and water
  5. filtrationfiltered through Celite
  6. extractionThe aqueous phase was extracted with EtOAc
  7. dry with materialThe combined organic layers were dried with MgSO4
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column