تفاعل #44486

ord-e58910d5be334e0b8fdc14a5c87f8aa6

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was evaporated in vacuo
  2. 2
    workup.STIRRINGstirred at room temperature for two hours
  3. 3
    أخرىThe reaction was quenched with 10% sodium bisulfite
  4. 4
    استخلاصextracted with dichloromethane
  5. 5
    غسيلThe organic phase was washed with water
  6. 6
    تجفيفdried with MgSO4
  7. 7
    ترشيحfiltered
  8. 8
    أخرىevaporated in vacuo

الإجراء التجريبي

To a solution of Example 1D (0.168 mg, 0.475 mmoles) in methanol (1.5 mL), two drops of 12M HCl was added and stirred for one hour. The solvent was evaporated in vacuo. The residue was taken in dichloromethane (2.5 mL) and Dess-Martin periodinane (0.25 gm, 0.593 mmoles) was added and stirred at room temperature for two hours. The reaction was quenched with 10% sodium bisulfite and extracted with dichloromethane. The organic phase was washed with water, dried with MgSO4, filtered, and evaporated in vacuo to provide the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737137B2uspto-grants-2010_06