반응 #717600

ord-b0d898fe99ca41dcbd16a289f92af956

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The precipitate was filtered
  2. 2
    세척washed with ether
  3. 3
    workup.DISSOLUTIONThen was dissolved with bicarbonate 4%
  4. 4
    추출extracted with ethyl acetate
  5. 5
    세척The organic layer was washed with brine
  6. 6
    기타dried
  7. 7
    기타the solvent was removed under reduced pressure

실험 절차

To a solution of methyl 4-amino-2-methoxybenzoate (13 g, 0.07 mol) in acetic acid (300 mL) was added dropwise a solution of iodine monochloride (11.5 g, 0.07 mol) in acetic acid (50 mL). The mixture was stirred for 1.5 hours at room temperature. The precipitate was filtered and washed with ether. Then was dissolved with bicarbonate 4% and extracted with ethyl acetate. The organic layer was washed with brine, dried and the solvent was removed under reduced pressure giving the title compound as a white solid (88%), which was used in the next step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09315463B2uspto-grants-2016_04