HRID853008

反应详情

EQUATION

反应方程式

HRID 853008 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of butyl (4-chloro-quinolin-6-ylmethylene)-amine (322 mg, 1.3 mmol) and a solution of sodium butoxide in butanol (3 mL, 6.0 mmol, 2.0M) were placed in a microwave tube and the mixture was heated to 120° C. for 30 min in a closed microwave. Then, the suspension was diluted with 3.0N hydrochloric acid (3 mL) and the solvent was removed under the vacuum. The residue was diluted with water and the organic compound was extracted into ethyl acetate (3×50 mL). The combined extracts were washed with saturated sodium bicarbonate solution, brine solution and dried over anhydrous magnesium sulfate. After filtration of the drying agent, the solvent was removed under the vacuum and the residue was purified by using a Biotage silica gel column chromatography to obtain 145 mg (48.5% yield) of 4-butoxy-quinoline-6-carbaldehyde as a white solid: EI-LRMS m/e calcd for C14H15NO2 (M+) 230.1, found 230.1.

WORKUP

后处理

  1. customthe solvent was removed under the vacuum
  2. additionThe residue was diluted with water
  3. extractionthe organic compound was extracted into ethyl acetate (3×50 mL)
  4. washThe combined extracts were washed with saturated sodium bicarbonate solution, brine solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationAfter filtration of the drying agent
  7. customthe solvent was removed under the vacuum
  8. customthe residue was purified