반응 #95376

ord-1d512c92792f43509a09120bf02ffcbe

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONTo the solution was added
  2. 2
    온도The mixture was refluxed
  3. 3
    농축the reaction solution was concentrated
  4. 4
    workup.ADDITIONTo the concentrate was added n-hexane (5 ml)
  5. 5
    기타crystallization of the reaction product
  6. 6
    여과The resulting product was recovered by filtration
  7. 7
    세척washed with n-hexan
  8. 8
    기타dried

실험 절차

6,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carboxylic acid (57.3 mg) was dissolved in benzene (10 ml). To the solution was added with stirring at room temperature thionyl chloride (0.5 ml). The mixture was refluxed with stirring for three hours, and the reaction solution was concentrated. To the concentrate was added n-hexane (5 ml) to cause crystallization of the reaction product. The resulting product was recovered by filtration and washed with n-hexan and dried. There were thus obtained 34.8 mg of the desired product (34.8 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04344944uspto-grants-1982_08