تفاعل #90092

ord-f865c7d0fe7f44da81d69c156db8f76c

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    استخلاصextracted with ethyl acetate
  2. 2
    استخلاصextracted with ethyl acetate
  3. 3
    غسيلwashed with saturated brine
  4. 4
    تجفيفdried over sodium sulfate
  5. 5
    أخرىThe drying agent was removed by filtration
  6. 6
    أخرىthe residues obtained
  7. 7
    تركيزafter concentration under reduced pressure
  8. 8
    أخرىwere purified by silica gel column chromatography (ethyl acetate/hexane)
  9. 9
    أخرىto obtain the target compound (white solid, 1.10 g, 84%)

الإجراء التجريبي

2-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid ethyl ester (Compound L3-1, 1.45 g, 5.17 mmol) was dissolved in THF (13 mL) and EtOH (13 mL), added with 1 N aqueous solution of sodium hydroxide (10.3 mL, 2.0 eq.), and stirred at 80° C. overnight. The reaction solution was added to water and extracted with ethyl acetate. The aqueous layer was acidified by using 1 N aqueous solution of hydrochloric acid, extracted with ethyl acetate, washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the target compound (white solid, 1.10 g, 84%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09440922B2uspto-grants-2016_09