HRID1074444

反应详情

EQUATION

反应方程式

HRID 1074444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2.2 g of sodium hydride (as a 50% oil dispersion) and 15.5 g of methyl iodide in 300 ml of dried dimethylformamide, there was added dropwise a solution of 7.1 g of 2-(4-nitrophenyl)butanol in 100 ml of dimethylformamide. The resulting mixture was stirred at room temperature for 20 hours and then poured into an aqueous solution containing 0.2 M potassium hydrogen phosphate/potassium dihydrogen phosphate buffer solution (pH 7). The resulting mixture was extracted several times with diethyl ether and the combined organic extracts were washed with aqueous dilute sodium thiosulfate solution, water, and aqueous saturated sodium chloride solution, and dried over magnesium sulfate. Evaporation of the solvent gave a red oil which was purified by chromatography on silica gel and elution with ethyl acetate/hexane to give 4-[1-(methoxymethyl)-propyl]nitrobenzene.

WORKUP

后处理

  1. additionpoured into an aqueous solution
  2. extractionThe resulting mixture was extracted several times with diethyl ether
  3. washthe combined organic extracts were washed with aqueous dilute sodium thiosulfate solution, water, and aqueous saturated sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. customEvaporation of the solvent
  6. customgave a red oil which
  7. customwas purified by chromatography on silica gel and elution with ethyl acetate/hexane