HRID1391732

反应详情

EQUATION

反应方程式

HRID 1391732 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Borane (10.80 mL of a 1M solution in THF, 10.80 mmol) was added to a cooled solution of 5-bromo-2-methyl-benzoic acid (116 mg, 0.54 mmol) in THF (15 mL), under nitrogen, at 0° C. (ice water bath) and the resulting mixture allowed to warm to rt overnight. The mixture was then treated with MeOH (10 mL) followed by aqueous HCl (2M, 20 mL) and the mixture stirred for about 15 minutes, concentrated under vacuum and then partitioned with EtOAc. The organic layer was washed with aqueous HCl (2M), water and brine, dried (MgSO4), filtered and reduced to give the title compound as a colourless oil (90 mg).

WORKUP

后处理

  1. concentrationconcentrated under vacuum
  2. custompartitioned with EtOAc
  3. washThe organic layer was washed with aqueous HCl (2M), water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered