反应 #9317

ord-9482f3b28cc4406ca403d81c37c7da8b

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤the organic layer was washed with brine
  2. 2
    干燥dried over anhydrous magnesium sulfate
  3. 3
    浓缩concentrated under reduced pressure

实验过程

After adding ethanol (2 μL), triphenylphosphine (15 mg) and diethyl azodicarboxylate (9 μL) to a solution of 2-[3-[di(cyclopropylmethyl)amino]-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-7-yl]-3,5-dimethylphenol (15 mg) in tetrahydrofuran (0.45 mL) under a nitrogen atmosphere, the mixture was stirred at room temperature overnight. The reaction mixture was added to water, extraction was performed with ethyl acetate, and the organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was subjected to silica gel column chromatography, and the title compound (3.7 mg) was obtained from the n-hexane:ethyl acetate (9:1) fraction as a yellow oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07091215B2uspto-grants-2006_08