반응 #360943

ord-f5aea3c16def4f2c9c9c9c482b76b49d

시약

없음

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to maintain the reaction temperature below 5° C
  2. 2
    농축The mixture was concentrated in vacuo to a brown solid
  3. 3
    기타the solid triturated with methanol
  4. 4
    여과The resulting white solid was collected by filtration

실험 절차

A solution of 15 g (86 mmole) of 2-phenylcyclohexanone in 60 mL of carbon tetrachloride at -5° C. was treated via rapid dropwise addition with a solution of 14.4 g (90 mmole) of bromine in 70 mL of carbon tetrachloride so as to maintain the reaction temperature below 5° C. The color disappeared rapidly. The mixture was concentrated in vacuo to a brown solid and the solid triturated with methanol. The resulting white solid was collected by filtration to provide 9.55 g of product. After cooling the mother liquor at -25° C., an additional 5.2 g of solid was obtained, for a total yield of 68%, a portion of which was carried on directly in Step B below.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05387595uspto-grants-1995_02