HRID81690

反应详情

EQUATION

反应方程式

HRID 81690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Crude methyl 4,5-dichloro-6-methylnicotinate (380 mg) was dissolved in 3 ml of methanol and, in a nitrogen stream, sodium methoxide (120 mg) was then added to the solution under cooling on ice. The temperature of the reaction solution was gradually raised to room temperature, and it was stirred for 18 hours. After the disappearance of the materials had been confirmed, a saturated ammonium chloride aqueous solution was added to the reaction solution under cooling on ice, followed by extraction with chloroform. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away. The residue was purified by silica gel chromatography (ethyl acetate-hexane), so as to obtain the title compound (210 mg) as a solid.

WORKUP

后处理

  1. additionwas then added to the solution
  2. temperatureunder cooling on ice
  3. temperatureunder cooling on ice
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. distillationthe solvent was then distilled away
  7. customThe residue was purified by silica gel chromatography (ethyl acetate-hexane)