HRID1647057

反应详情

EQUATION

反应方程式

HRID 1647057 的结构方程式

PROCEDURE

实验过程

A mixture of 5-[(4-bromophenyl)methyl]-2H-tetrazole (18.5 g, 77 mmol), t-butanol (11.4 g, 150 mmol), trifluoroacetic acid (76 mL, 1.0 mol) and concentrated sulfuric acid (3.8 g, 39 mmol) was stirred for 24 h and then partitioned between ethyl acetate (250 mL) and water (100 mL). The organic layer was washed with water (4×100 mL) and 1M NaOH (2×100 mL) and was dried over sodium sulfate. Filtration and removal of the solvent in vacuo produced a solid that was recrystallized from hexane to give 5-[(4-bromophenyl)methyl]-2-(1,1-dimethylethyl)-2H-tetrazole. (12.3 g, 47 mmol) in 54% yield, mp. 69°-70° C.

WORKUP

后处理

  1. custompartitioned between ethyl acetate (250 mL) and water (100 mL)
  2. washThe organic layer was washed with water (4×100 mL) and 1M NaOH (2×100 mL)
  3. dry with materialwas dried over sodium sulfate
  4. filtrationFiltration and removal of the solvent in vacuo
  5. customproduced a solid
  6. customthat was recrystallized from hexane