HRID340449

反应详情

EQUATION

反应方程式

HRID 340449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A DMF (2 ml) solution containing 3-bromoquinolin-8-amine (223 mg), dimethyl sulfate (189 mg), potassium carbonate (415 mg), and sodium iodide (20 mg) were added to a tube and the tube was sealed, followed by stirring at 95° C. for 17 hours. The reaction solution was cooled to room temperature, ethyl acetate was added, an insoluble precipitate was removed, and the organic layer was washed with 1M hydrochloric acid, water, and saturated saline. Subsequently, the organic layer was dried over anhydrous sodium sulfate, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=0:1 to 1:1), and a yellow solid of 3-bromo-N-methylquinolin-8-amine (52 mg) was thus obtained.

WORKUP

后处理

  1. additionwere added to a tube
  2. customthe tube was sealed
  3. temperatureThe reaction solution was cooled to room temperature
  4. customan insoluble precipitate was removed
  5. washthe organic layer was washed with 1M hydrochloric acid, water, and saturated saline
  6. dry with materialSubsequently, the organic layer was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled away under reduced pressure
  8. customthe obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=0:1 to 1:1)