반응 #2030163

ord-99fed4c2c183480e86dca7e96e9a731b

반응 방정식

c1ccc(-c2c3ccccc3cc3ccccc23)cc1
9-phenylanthracene
BrBr
bromine
O=S([O-])([O-])=S.[Na+].[Na+]
sodium thiosulfate
Brc1c2ccccc2c(-c2ccccc2)c2ccccc12
10-bromo-9-phenylanthracene

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was dripped through a dropping funnel into the reaction solution
  2. 2
    기타After the reaction
  3. 3
    기타the reaction
  4. 4
    세척An organic layer was washed with a sodium hydroxide (NaOH) aqueous solution
  5. 5
    건조a saturated saline solution and dried with magnesium sulfate
  6. 6
    여과After the solution was filtered naturally
  7. 7
    농축the filtrate was concentrated
  8. 8
    workup.DISSOLUTIONdissolved in toluene
  9. 9
    여과filtered through Florisil, Celite, and alumina
  10. 10
    농축When the filtrate was concentrated
  11. 11
    기타recrystallized with dichloromethane and hexane, 7.0 g of a light yellow solid of 10-bromo-9-phenylanthracene that
  12. 12
    기타was obtained (yield: 89%)

실험 절차

After 6.0 g (23.7 mmol) of 9-phenylanthracene was dissolved in 80 mL of carbon tetrachloride, a solution of 3.80 g (21.1 mmol) of bromine dissolved in 10 mL of carbon tetrachloride was dripped through a dropping funnel into the reaction solution. After the dripping, the solution was stirred at room temperature for one hour. After the reaction, a sodium thiosulfate aqueous solution was added to stop the reaction. An organic layer was washed with a sodium hydroxide (NaOH) aqueous solution and a saturated saline solution and dried with magnesium sulfate. After the solution was filtered naturally, the filtrate was concentrated, dissolved in toluene, and filtered through Florisil, Celite, and alumina. When the filtrate was concentrated and recrystallized with dichloromethane and hexane, 7.0 g of a light yellow solid of 10-bromo-9-phenylanthracene that was an object was obtained (yield: 89%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08389735B2uspto-grants-2013_03