反应 #43915

ord-3b485b6a866c42c08a921b338e281176

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooled
  2. 2
    萃取extracted with ethyl acetate
  3. 3
    洗涤The extract was washed with saturated brine
  4. 4
    干燥dried over anhydrous magnesium sulfate
  5. 5
    浓缩concentrated under reduced pressure
  6. 6
    其他The obtained crystals were recrystallized from heptane-ethyl acetate

实验过程

A solution of 2′,6′-dimethyl-4′-[3-(methylsulfonyl)propoxy]biphenyl-3-carbaldehyde (2.66 g, 7.68 mmol) in a mixed solvent of methanol (10 mL) and tetrahydrofuran (20 mL) was ice-cooled, sodium borohydride (90%, 0.323 g, 7.68 mmol) was added, and the mixture was stirred for 6 hr under nitrogen atmosphere. The reaction mixture was treated with diluted hydrochloric acid, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained crystals were recrystallized from heptane-ethyl acetate to give the title compound (2.60 g, yield 97%) as colorless crystals.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07732626B2uspto-grants-2010_06