HRID467958

反应详情

EQUATION

反应方程式

HRID 467958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of N-[3-(trifluoromethoxy)benzyl]tetrahydro-2H-pyran-4-amine (450 mg), 1-methyl-1H-imidazole-4-carboxylic acid (210 mg), EDC.HCl (320 mg), HOBt (250 mg) and acetonitrile (5 mL) was stirred at room temperature for an hour. Acetonitrile was distilled off under reduced pressure and an aqueous solution of 6 M sodium hydroxide was added. Extraction was conducted with ethyl acetate and the solvent was concentrated. The residue was purified by column chromatography (NH silica gel cartridge; ethyl acetate) to give the titled compound (90 mg).

WORKUP

后处理

  1. distillationAcetonitrile was distilled off under reduced pressure
  2. additionan aqueous solution of 6 M sodium hydroxide was added
  3. extractionExtraction
  4. concentrationthe solvent was concentrated
  5. customThe residue was purified by column chromatography (NH silica gel cartridge; ethyl acetate)