반응 #4586
ord-42d1b3eddfb84c7aa01824183c097731
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타the pale yellow solid which formed
- 2기타was collected
- 3workup.DISSOLUTIONdissolved in water
- 4기타On acidification of the solution to pH 1, a precipitate formed which
- 5기타was collected
- 6기타recrystallized 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.