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Hydrogen Peroxide → 9h-Fluoren-2-yl acetate

HRID 2416351
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HRID 2416351 반응식
S(=O)(=O)(O)O.C([C:9]1[CH:21]=[CH:20][C:19]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH2:12][C:11]=2[CH:10]=1)(=O)C.[C:22]([O:25]C(=O)C)(=[O:24])[CH3:23].OO>O.C(O)=O>[C:22]([O:25][C:9]1[CH:21]=[CH:20][C:19]2[C:14]3[C:13](=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:12][C:11]=2[CH:10]=1)(=[O:24])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 699082-Acetylfluorene

생성물 1

HCID 2470609h-Fluoren-2-yl acetate수율 83.9%

시약·촉매·용매 2

HCID 284Formic Acid용매
HCID 962
Water
용매

실험 절차

Sulfuric acid (40 mL) was added to a mixture of 2-acetylfluorene (165 g), formic acid (320 g), acetic anhydride (120 g) and dicholoromethane (1 L), and then aqueous hydrogen peroxide (120 mL) was dropwise added thereto. The solution was stirred for 30 minutes at a room temperature, and it was heated up to 40° C. and further stirred for 5 hours. Water (1 L) was added to the reaction mixture, and the dichloromethane layer was separated. The dichloromethane layer was washed in order with a saturated sodium carbonate aqueous solution, a sodium hydrogensulfite aqueous solution and water, and then it was dried on anhydrous magnesium sulfate and concentrated to obtain a solid matter. This was recrystallized from a mixed solvent of heptane-ethyl acetate (1:1) to obtain 2-acetoxyfluorene (149 g) of colorless needle crystal. The melting point was 130 C.

후처리

  1. temperatureit was heated up to 40° C.
  2. stirringfurther stirred for 5 hours
  3. customthe dichloromethane layer was separated
  4. washThe dichloromethane layer was washed in order with a saturated sodium carbonate aqueous solution
  5. dry with materiala sodium hydrogensulfite aqueous solution and water, and then it was dried on anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto obtain a solid matter
  8. customThis was recrystallized from a mixed solvent of heptane-ethyl acetate (1:1)

출처 및 근거

ORD 기록
ord-0ea5664139024967b164e558b7400518
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06824709B2

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