반응 #345555

ord-580cc170fb7d4f6db281576fdfd83fb5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타In a flask were combined
  2. 2
    여과It was then filtered
  3. 3
    기타the methyl ethyl ketone removed in vacuo
  4. 4
    기타The solids recovered from the filter
  5. 5
    추출were extracted with acetone
  6. 6
    workup.DISSOLUTIONThe combined solids were dissolved in water
  7. 7
    기타The solvents were removed in vacuo
  8. 8
    기타producing

실험 절차

In a flask were combined 3.0 grams (g) (25.4 mmol) phenyl cyanamide, 1.83 g (25.4 mmol) 1,2-epoxy butane, 3.51 g (25.4 mmol) potassium carbonate and 50 milliliters (ml) methyl ethyl ketone. The mixture was stirred overnight under a nitrogen blanket at room temperature. It was then filtered and the methyl ethyl ketone removed in vacuo. The solids recovered from the filter were extracted with acetone and combined with the residue from the main portion. The combined solids were dissolved in water and extraced with 15% isopropanol in chloroform. The solvents were removed in vacuo producing 2.30 g (48% of theoretical yield) of the desired product. Spectroscopic analysis confirmed the structure of the desired product. No type II product was detected.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05266701uspto-grants-1993_11