تفاعل #74835

ord-b7a1a5518949456f9e3d128f0626a445

الكواشف

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ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONTo a mixture of 68.5 g
  2. 2
    درجة الحرارةrefluxed on a steam bath for 6 hours
  3. 3
    workup.STIRRINGstirred overnight at room temperature
  4. 4
    ترشيحthe mixture is filtered
  5. 5
    workup.DISSOLUTIONThe solid is dissolved in warm ethyl acetate
  6. 6
    ترشيحfiltered
  7. 7
    أخرىThe filtrate is evaporated to a solid

الإجراء التجريبي

To a mixture of 68.5 g. of p-chlorobenzonitrile and 24.0 g. of sodium hydride (50% in mineral oil) in 250 ml. of ether is added, 26.1 ml. of acetonitrile and 2 ml. of isopropanol. The mixture is stirred and refluxed on a steam bath for 6 hours and then stirred overnight at room temperature. A 5 ml. portion of methanol and 250 ml. of water are added. The ether is boiled away on a steam bath and the mixture is filtered. The solid is dissolved in warm ethyl acetate and filtered. The filtrate is evaporated to a solid giving β-amino-4-chlorocinnamonitrile.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04173650uspto-grants-1979_11