تفاعل #9221

ord-74007a0173b8457e84bcfc9f8de348a6

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe precipitate was filtered off
  2. 2
    غسيلwashed with Et2O
  3. 3
    أخرىa new precipitate was formed
  4. 4
    ترشيحIt was filtered off
  5. 5
    غسيلwashed with water and MeOH
  6. 6
    أخرىdried under vacuum

الإجراء التجريبي

A solution of 4-benzylaniline (0.916 g, 5.00 mmol) and KSCN (0.97 g, 10.0 mmol, 2.0 eq) in 10 mL acetic acid was cooled at about 5° C., and was treated dropwise with a solution of bromine (0.258 mL, 5.00 mmol, 1.0 eq) in 2 mL acetic acid. The mixture was stirred at room temperature for about 1 hour. The precipitate was filtered off and washed with Et2O. The obtained solid was neutralized with saturated sodium carbonate solution, and a new precipitate was formed. It was filtered off, washed with water and MeOH, and dried under vacuum to give the desired compound 1.06 g (88%). LC/MS 241.2 (M+1); LC retention time 2.46 min.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091227B2uspto-grants-2006_08