HRID1060864

反应详情

EQUATION

反应方程式

HRID 1060864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-[2-methyl-8-2,4,6-trimethyl-phenyl)quinolin4-yl]-propan-1-one (52 mg), iso-butoxylamine hydrochloride (300 mg), potassium carbonate (50 mg) and sodium acetate (40 mg) in ethanol (2 ml) was stirred at room temperature for 48 hr. The mixture was concentrated to dryness, then diluted with water, brine, and extracted with chloroform. The organic layer was separated, dried (Na2SO4) and concentrated to dryness to give a mixture of the title (Z) and (E)-isomer, respectively. The crude mixture was purified by preparative thin layer chromatography with 7% ethyl acetate in hexane as solvent to give a 6:4 mixture of isomers.

WORKUP

后处理

  1. concentrationThe mixture was concentrated to dryness
  2. additiondiluted with water, brine
  3. extractionextracted with chloroform
  4. customThe organic layer was separated
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated to dryness
  7. customto give
  8. customThe crude mixture was purified by preparative thin layer chromatography with 7% ethyl acetate in hexane as solvent
  9. customto give
  10. additiona 6:4 mixture of isomers