تفاعل #47417

ord-bb14228bf7204204a4fa539d2683da72

المذيبات

ظروف التفاعل

درجة الحرارة
15°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe solvents evaporated
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in water
  3. 3
    غسيلwashed with diethyl ether
  4. 4
    استخلاصextracted with ethyl acetate
  5. 5
    تجفيفThe combined organic layers were dried over sodium sulfate
  6. 6
    تركيزconcentrated

الإجراء التجريبي

To a solution containing (S)-2-[4-(3-bromo-2-fluoro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methyl-pentanoic acid ethyl ester (0.260 g, 0.63 mmol) in tetrahydrofuran (8 mL) was treated with an aqueous solution of lithium hydroxide monohydrate (0.5N, 3 mL, 1.5 mmol). The mixture was stirred at 15° C. for 3 h, and the solvents evaporated. The residue was dissolved in water and washed with diethyl ether, and the diethyl ether layer discarded. The aqueous phase was acidified with dilute hydrochloric acid (pH <2), and extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and concentrated to afford (S)-2-[4-(3-bromo-2-fluoro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methyl-pentanoic acid, (0.250 g, 100%), as a yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741327B2uspto-grants-2010_06