반응 #360943
ord-f5aea3c16def4f2c9c9c9c482b76b49d
시약
없음
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도to maintain the reaction temperature below 5° C
- 2농축The mixture was concentrated in vacuo to a brown solid
- 3기타the solid triturated with methanol
- 4여과The 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.