HRID1518065

反应详情

EQUATION

反应方程式

HRID 1518065 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NaBH4 (1.2 g, 64 mmol) is added portionwise slowly to an EtOH (100 mL) solution of crude 2-methyl-N-[3,5-bis(trifluoromethyl)phenylmethylene]-2H-tetrazole-5-amine at 0° C., and the mixture is stirred at room temperature for 1 hour. After addition of sat. NH4Cl aq. and water at 0° C., the mixture is extracted with EtOAc. The combined organic layer is washed with brine, dried over magnesium sulfate, filtered and concentrated The residue is purified by silica gel column chromatography chromatography to give N-[3,5-bis(trifluoromethyl)benzyl]-N-(2-methyl-2H-tetrazol-5-yl)amine as a white crystalline solid.

WORKUP

后处理

  1. extractionthe mixture is extracted with EtOAc
  2. washThe combined organic layer is washed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated The residue
  6. customis purified by silica gel column chromatography chromatography