反应详情

NaBH4 (8.2 g, 0.22 mol) is added portionwise slowly to EtOH (700 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 concentrated to remove 300 mL of EtOH and extracted with CH2Cl2 (300 mL×4 times). The combined organic layer is washed with brine, dried over magnesium sulfate, filtered and concentrated The residue is purified by silica gel column chromatography to give N-[3,5-bis(trifluoromethyl)benzyl]-N-(2-methyl-2H-tetrazol-5-yl)amine as a white crystalline solid.

1. concentrationthe mixture is concentrated
2. customto remove 300 mL of EtOH
3. extractionextracted with CH2Cl2 (300 mL×4 times)
4. washThe combined organic layer is washed with brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated The residue
8. customis purified by silica gel column chromatography