HRID2236834

反应详情

EQUATION

反应方程式

HRID 2236834 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 0° C. mixture of [1-(4-nitro-phenyl)-piperidin-4-yl]-methanol and iodomethane (0.25 mL, 4.0 mmol) in N,N-dimethylformamide (3 mL) is added sodium hydride (60% dispersion in mineral oil, 80 mg, 2.0 mmol). The cooling bath is removed and the mixture is stirred at room temperature for five hours before it is re-cooled to 0° C. and quenched by the addition of saturated aqueous sodium hydrogen carbonate solution. The precipitated solid is collected by Büchner filtration, washed with water, and dried under house vacuum to give 4-methoxymethyl-1-(4-nitro-phenyl)-piperidine as pale yellow crystals (0.15 g, 60%).

WORKUP

后处理

  1. customThe cooling bath is removed
  2. temperatureis re-cooled to 0° C.
  3. customquenched by the addition of saturated aqueous sodium hydrogen carbonate solution
  4. filtrationThe precipitated solid is collected by Büchner filtration
  5. washwashed with water
  6. customdried under house vacuum