تفاعل #159639

ord-81d088ce54304cf29e2e7ba529ec83ca

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةunder reflux overnight
  3. 3
    تركيزthe mixture was concentrated in vacuo
  4. 4
    workup.ADDITIONThe residue was diluted with water (10 ml)
  5. 5
    استخلاصthe resulting mixture was extracted with ethyl acetate (2×10 ml)
  6. 6
    غسيلThe organic solution was washed with brine (20 ml)
  7. 7
    تجفيفdried over Na2SO4
  8. 8
    أخرىevaporated in vacuo

الإجراء التجريبي

To an ice cooled solution of methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate (D72) (165 mg, 0.520 mmol) in methanol (10 ml), 10N NaOH (10 ml) was added. The mixture was heated under reflux overnight. After cooled to room temperature, the mixture was concentrated in vacuo. The residue was diluted with water (10 ml), acidified with 2.5N HCl (pH 1-2), and the resulting mixture was extracted with ethyl acetate (2×10 ml). The organic solution was washed with brine (20 ml), dried over Na2SO4 and evaporated in vacuo to afford the title compound (D98) (170 mg) as a red solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08828987B2uspto-grants-2014_09