تفاعل #6896

ord-941df1acbb1249ef9c18b030f6937c2a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe resulting mixture was degassed
  2. 2
    ترشيحThe reaction mixture was filtered
  3. 3
    ترشيحthrough filter aid
  4. 4
    أخرىthe solvent removed under vacuum
  5. 5
    workup.DISSOLUTIONThe resulting oil was dissolved in ethyl acetate
  6. 6
    أخرىthe solvent removed under vacuum
  7. 7
    أخرىtriturated until crystallization
  8. 8
    ترشيحThe solids were filtered
  9. 9
    غسيلwashed with ice-cold ether
  10. 10
    أخرىthen dried under vacuum

الإجراء التجريبي

The product of Step A and palladium hydroxide on carbon (1.3 g, 20% by wt) was suspended in methanol (100 mL) and ethyl acetate (100 mL). The resulting mixture was degassed then stirred under hydrogen atmosphere (balloon) for 6 h. The reaction mixture was filtered through filter aid and the solvent removed under vacuum. The resulting oil was dissolved in ethyl acetate and the solvent removed under vacuum. The resulting oil was suspended in ether and triturated until crystallization occurred. The solids were filtered and washed with ice-cold ether then dried under vacuum to afford the product as a brown solid, MS: m/z 254 (MH+), which was used without further purification

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07084156B2uspto-grants-2006_08