تفاعل #796941

ord-c1f953ee49e7433da0a0a76540785fc8

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe mixture was extracted with ethyl acetate
  2. 2
    غسيلThe extract was washed with water and saturated brine
  3. 3
    تجفيفdried over anhydrous magnesium sulfate
  4. 4
    ترشيحAfter silica gel filtration
  5. 5
    أخرىthe solvent was evaporated under reduced pressure

الإجراء التجريبي

Under a nitrogen atmosphere, to a solution of methyl 5-hydroxynicotinate (5.00 g) in DMF (50 mL) were added isobutyl bromide (5.33 mL) and potassium carbonate (9.04 g), and the mixture was stirred at 80° C. for 2 hr. Water was added to the reaction mixture at room temperature, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. After silica gel filtration, the solvent was evaporated under reduced pressure to give a crude product of the title compound (5.13 g) as a pale-brown oil. The obtained crude product was directly used for the next step.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09181186B2uspto-grants-2015_11