反应 #1914851

ord-51cbbc77137b4f26ad2abe29e4d50d5a

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooled on an ice bath
  2. 2
    其他The solvent was evaporated
  3. 3
    其他the residue was partitioned between diethyl ether and aqueous sodium bicarbonate
  4. 4
    洗涤The ethereal layer was washed with more aqueous sodium bicarbonate and brine
  5. 5
    干燥dried (Na2SO4)
  6. 6
    其他evaporated
  7. 7
    其他The crude product crystallised soon
  8. 8
    其他could be used without further purification

实验过程

2,6-Difluoro-4-formylbenzonitrile (1.36 g, 8.13 mmol; see step (x) above) was dissolved in 25 mL of methanol and cooled on an ice bath. Sodium borohydride (0.307 g, 8.12 mmol) was added in portions with stirring and the reaction was left for 65 min. The solvent was evaporated and the residue was partitioned between diethyl ether and aqueous sodium bicarbonate. The ethereal layer was washed with more aqueous sodium bicarbonate and brine, dried (Na2SO4) and evaporated. The crude product crystallised soon and could be used without further purification. Yield: 1.24 g (90%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07056907B2uspto-grants-2006_06