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Sodium Hydroxide → Benzonorbornadienone

HRID 1586722
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HRID 1586722 반응식
[C:1]12[CH2:7][C:4](=[CH:5][CH:6]=1)[C:3]1[CH:8]=[CH:9][CH:10]=[CH:11][C:2]2=1.[OH-:12].[Na+].[BH4-].[Na+]>O.O1CCCC1>[C:4]12[C:5](=[O:12])[CH:6]=[C:1]([CH:7]=1)[C:2]1[CH:11]=[CH:10][CH:9]=[CH:8][C:3]2=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 566125711,4-Methanonaphthalene

생성물 1

HCID 129692535Benzonorbornadienone

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

실험 절차

A solution of mercuric acetate (4 g) in water (10 ml) was treated with a solution of benzobicyclo[2.2.1]heptadiene (2 g) in tetrahydrofuran (25 ml) and the resulting mixture was stirred at room temperature for 24 hours. The solution was treated with a solution of 10% sodium hydroxide in water (5 ml), followed by sodium borohydride (0.5 g). The resulting mixture was stirred for 30 minutes and the resulting layers were separated. The aqueous layer was extracted with ether (2×30 ml) and the combined organic layers were dried over magnesium sulfate and concentrated on a rotary evaporator. The residue was combined with methylene chloride (25 ml) and pyridinium chlorochromate (3 g) and the solution was stirred at room temperature for 12 hours. The solution was washed with water (30 ml) and the organic layer was dried over magnesium sulfate. The solvent was removed on a rotary evaporator and the product was purified by preparative centrifugally accelerated radial thin layer chromatography using 25% ethyl acetate in hexane as the eluant. After removal of the eluant on a rotary evaporator, the product was obtained as a yellow oil.

후처리

  1. stirringThe resulting mixture was stirred for 30 minutes
  2. customthe resulting layers were separated
  3. extractionThe aqueous layer was extracted with ether (2×30 ml)
  4. dry with materialthe combined organic layers were dried over magnesium sulfate
  5. concentrationconcentrated on a rotary evaporator
  6. stirringthe solution was stirred at room temperature for 12 hours
  7. washThe solution was washed with water (30 ml)
  8. dry with materialthe organic layer was dried over magnesium sulfate
  9. customThe solvent was removed on a rotary evaporator
  10. customthe product was purified by preparative centrifugally accelerated radial thin layer chromatography
  11. customAfter removal of the eluant
  12. customon a rotary evaporator
  13. customthe product was obtained as a yellow oil

출처 및 근거

ORD 기록
ord-91839184b74f4398b40336aef078c6af
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05215992

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