تفاعل #481827

ord-b6b1c39d689e463eb8b07615daf0c5b5

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe DMF is then evaporated
  2. 2
    غسيلWashing with ethyl acetate and with water
  3. 3
    أخرىthe two phases are separated
  4. 4
    تجفيفThe combined organic phases are dried over MgSO4
  5. 5
    أخرىthe solvent is evaporated
  6. 6
    أخرىThe oil obtained
  7. 7
    أخرىis purified on a silica column (eluant: PE/AcOEt 8/2), which
  8. 8
    أخرىto be obtained

الإجراء التجريبي

3 g (18.05 mmol) of the alcohol obtained in Step A are dissolved in 10 ml of DMF in a flask. 2 eq. of NaH (60% in oil) are added slowly and allowed to act for 30 minutes under an inert atmosphere. 2 eq. of iodomethane are then added. The mixture is stirred for 2 hours; the DMF is then evaporated. Washing with ethyl acetate and with water is carried out and the two phases are separated. The combined organic phases are dried over MgSO4 and the solvent is evaporated. The oil obtained is purified on a silica column (eluant: PE/AcOEt 8/2), which allows the pure title product to be obtained.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06602903B2uspto-grants-2003_08