تفاعل #167769

ord-149984a2e97141098b22c88ceba91bee

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    تركيزThe reaction solution was concentrated
  3. 3
    workup.ADDITIONthe residue was diluted with ethyl acetate
  4. 4
    workup.ADDITIONTo this solution, a 1M hydrochloric acid in acetic acid solution was added
  5. 5
    workup.STIRRINGthe mixture was stirred
  6. 6
    workup.ADDITIONFurther, diethyl ether was added
  7. 7
    ترشيحthe precipitated solid was collected by filtration

الإجراء التجريبي

To the compound 77a (523 mg) obtained at Step (1), 1M hydrochloric acid in acetic acid solution (18 ml) was added, and the mixture was stirred at room temperature for 2.5 hours. The reaction solution was concentrated, then the residue was diluted with ethyl acetate. To this solution, a 1M hydrochloric acid in acetic acid solution was added and the mixture was stirred. Further, diethyl ether was added, and the precipitated solid was collected by filtration to obtain the title compound (410 mg).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08846660B2uspto-grants-2014_09