Hydrochloric Acid → 1-(7-Ethyl-9H-fluoren-2-YL)ethan-1-one

HRID 1077304노트

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HRID 1077304 반응식
[C:1](OC(=O)C)(=[O:3])[CH3:2].[Cl-].[Al+3].[Cl-].[Cl-].[CH2:12]([C:14]1[CH:26]=[CH:25][C:24]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH2:17][C:16]=2[CH:15]=1)[CH3:13].Cl>ClC(Cl)C>[C:1]([C:20]1[CH:21]=[CH:22][C:23]2[C:24]3[C:16](=[CH:15][C:14]([CH2:12][CH3:13])=[CH:26][CH:25]=3)[CH2:17][C:18]=2[CH:19]=1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 2749392-Ethyl-9H-fluoreneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 215039081-(7-Ethyl-9H-fluoren-2-YL)ethan-1-one

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매3회

실험 절차

Acetic anhydride (2.67 g.) in dichloroethane (10 ml.) was added dropwise to a stirred, cooled (0°) suspension of aluminum chloride (6.95 g.) in dichloroethane (20 ml.). Cooling and stirring were continued during the dropwise addition of a solution of 2-ethylfluorene (4.61 g.) in dichloroethane (50 ml.). The mixture was stirred for one hour at room temperature and then decomposed by the dropwise addition of 2N-hydrochloric acid (40 ml.) to the cooled solution. The organic layer was separated, washed with water and with aqueous sodium bicarbonate, dried over anhydrous sodium sulphate, filtered, and evaporated under reduced pressure. The residue was recrystallised from light petroleum (ca 250 ml., b.p. 60°-80°) to give 2-acetyl-7-ethylfluorene m.p. 120°-122°.

후처리

  1. temperaturecooled
  2. temperatureCooling
  3. stirringThe mixture was stirred for one hour at room temperature
  4. customThe organic layer was separated
  5. washwashed with water and with aqueous sodium bicarbonate
  6. dry with materialdried over anhydrous sodium sulphate
  7. filtrationfiltered
  8. customevaporated under reduced pressure
  9. customThe residue was recrystallised from light petroleum (ca 250 ml., b.p. 60°-80°)

출처 및 근거

ORD 기록
ord-9e60e01118f34d20b67d204e025b32b2
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03959482

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