HRID34011

反应详情

EQUATION

反应方程式

HRID 34011 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 0.61 g of (2-chlorothiophen-3-yl)-(naphthalen-2-yl)-methanone in 6 mL of ethanol was added 0.12 mL of hydrazine monohydrate at room temperature and heated under reflux for 2 days. The reaction solution was diluted with ethyl acetate, and the organic layer washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The resultant crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30-1:5), to afford 32 mg of the title compound as colorless crystals.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 2 days
  3. washthe organic layer washed successively with saturated aqueous ammonium chloride and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated
  6. customThe resultant crude product was purified
  7. customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:30-1:5)