반응 #8539

ord-11ea0b2a940b4be2882a47ea40b946fa

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at 0° C
  2. 2
    기타the solvent was evaporated
  3. 3
    workup.ADDITIONAfter adding water
  4. 4
    세척the residue was washed with chloroform
  5. 5
    workup.ADDITIONNext, hydrochloric acid (6 mol/l) was slowly added to the aqueous layer until pH value
  6. 6
    추출Then the aqueous layer was extracted with IPE
  7. 7
    건조The organic layer was dried over anhydrous magnesium sulfate
  8. 8
    기타the solvent was evaporated

실험 절차

Ethyl 2-(2,3,4-trifluoroanilino)propionate (2.47 g) was dissolved in ethanol (40 ml) and an aqueous solution (3 mol/l; 10 ml) of sodium hydroxide was slowly added thereto at 0° C. After stirring at room temperature for 3 hours, the solvent was evaporated. After adding water, the residue was washed with chloroform. Next, hydrochloric acid (6 mol/l) was slowly added to the aqueous layer until pH value reached 1. Then the aqueous layer was extracted with IPE. The organic layer was dried over anhydrous magnesium sulfate and then the solvent was evaporated to give the title compound (2.19 g) as colorless crystals. Various spectral data of this product was identical with those obtained in Example 23.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087778B2uspto-grants-2006_08