تفاعل #44010

ord-53b29a51ccae49489e1545faedee3cbf

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwas quenched with sat. NaHCO3 (10 mL) and 10%
  2. 2
    workup.STIRRINGThe mixture was stirred at room temperature for 30 minutes
  3. 3
    استخلاصThe reaction mixture was extracted with CH2Cl2
  4. 4
    غسيلthe combined organic layers were washed with brine
  5. 5
    تجفيفThe organic layer was dried over Na2SO4
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated in vacuo

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07732609B2uspto-grants-2010_06