تفاعل #95376

ord-1d512c92792f43509a09120bf02ffcbe

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONTo the solution was added
  2. 2
    درجة الحرارةThe mixture was refluxed
  3. 3
    تركيزthe reaction solution was concentrated
  4. 4
    workup.ADDITIONTo the concentrate was added n-hexane (5 ml)
  5. 5
    أخرىcrystallization of the reaction product
  6. 6
    ترشيحThe resulting product was recovered by filtration
  7. 7
    غسيلwashed with n-hexan
  8. 8
    أخرىdried

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04344944uspto-grants-1982_08