HRID910765

反应详情

EQUATION

反应方程式

HRID 910765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of to 4,5-difluoro-2-nitrobenzoic acid (25.9 g) in THF (90 ml), cooled to 0° C., was carefully added borane-tetrahydrofuran complex (319 ml, 1M in THF). After the addition was complete, the mixture was stirred at 60° C. for 3 h. Methanol (150 ml) was added to the mixture at 0° C. and after 10 minutes the mixture was concentrated in vacuo. The residue was poured into water and extracted with ethyl acetate. The organic layer was washed with sat. aq. NaCl, dried (MgSO4), filtered and concentrated in vacuo.

WORKUP

后处理

  1. additionAfter the addition
  2. concentrationwas concentrated in vacuo
  3. additionThe residue was poured into water
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with sat. aq. NaCl
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo