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

HRID 1077304ノート

反応式

HRID 1077304 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒3 回

実験手順

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°.

後処理

  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°)

出典と根拠

ORDレコード
ord-9e60e01118f34d20b67d204e025b32b2
出典データセット
uspto-grants-1976_05
特許番号
US03959482

反応ノート

読み込み中…