反応 #44010

ord-53b29a51ccae49489e1545faedee3cbf

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was quenched with sat. NaHCO3 (10 mL) and 10%
  2. 2
    workup.STIRRINGThe mixture was stirred at room temperature for 30 minutes
  3. 3
    抽出The reaction mixture was extracted with CH2Cl2
  4. 4
    洗浄the combined organic layers were washed with brine
  5. 5
    乾燥The organic layer was dried over Na2SO4
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated in vacuo

実験手順

Compound 78 (0.50 g, 1.5 mmol) was dissolved in CH2Cl2 (5 mL). NaHCO3 (0.3 g, 3.6 mmol) was added, followed by Dess-Martin periodinane (0.78 g, 1.8 mmol). The reaction stirred at room temperature for two hours and was quenched with sat. NaHCO3 (10 mL) and 10% w/v sodium bisulfite (10 mL). The mixture was stirred at room temperature for 30 minutes. The reaction mixture was extracted with CH2Cl2 and the combined organic layers were washed with brine. The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo to yield 0.4 g of 79 as a white solid that was used without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07732609B2uspto-grants-2010_06