반응 #4586

ord-42d1b3eddfb84c7aa01824183c097731

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the pale yellow solid which formed
  2. 2
    기타was collected
  3. 3
    workup.DISSOLUTIONdissolved in water
  4. 4
    기타On acidification of the solution to pH 1, a precipitate formed which
  5. 5
    기타was collected
  6. 6
    기타recrystallized from ethyl acetate (EtOAc)/petroleum ether (30-60° C)

실험 절차

Benzoylcyanamide was prepared by the addition of benzoyl chloride (6.33 g, 0.045 mol) in 100 ml of diethyl ether to a suspension of monosodium cyanamide (5.76 g, 0.090 mol) in 100 ml of ether at 4° C. The reaction was stirred overnight at room temperature and the pale yellow solid which formed was collected and dissolved in water. On acidification of the solution to pH 1, a precipitate formed which was collected and recrystallized from ethyl acetate (EtOAc)/petroleum ether (30-60° C) to give 2 (5.89 g, 89.7% yield), mp 140°-142° C. [reported mp 139°-140° C⟧ Anal. Calcd for C8H6H2O: C, 65.75; H, 4.11; N, 19.18. Found: C, 65.79; H, 4.35; N, 19.04.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04726941uspto-grants-1988_02