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Acetone → 5-Fluoro-2,2-dimethylbenzo[d][1,3]dioxole

HRID 2226096
ノート
印刷プレビュー

反応式

HRID 2226096 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[OH:9].[CH3:10][C:11]([CH3:13])=O.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C(Cl)Cl>[CH3:10][C:11]1([CH3:13])[O:1][C:2]2[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=2[O:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 180AcetoneHCID 14812Phosphorus oxide (P4O10)HCID 1604584-Fluoro-1,2-benzenediol

生成物 1

HCID 189662825-Fluoro-2,2-dimethylbenzo[d][1,3]dioxole収率 56.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In a flask were placed 40 g (0.31 mole) of 1,2-dihydroxy-4-fluorobenzene, 36.25 g (0.625 mole) of acetone, and 400 mL of methylene chloride. To this solution was added 133 g (0.937 mole) of phosphorus pentoxide in portions during a five minute period. This mixture was stirred at ambient temperature for approximately 16 hours after which the methylene chloride was decanted from the solid material in the flask. Ice was added to the flask, and the solid residue was dissolved in water and extracted with methylene chloride. The phases were separated, and the organic phase was combined with the methylene chloride solution that had been decanted from the reaction mixture. This solution was washed in succession with a 5% aqueous solution of sodium hydroxide and then with water. After being dried over anhydrous magnesium sulfate and filtered, the organic solution was evaporated under reduced pressure, leaving 29.3 g of 2,2-dimethyl-5-fluoro-1,3-benzodioxole as a residue. The NMR spectrum was consistent with the proposed structure.

後処理

  1. customIn a flask were placed
  2. customwas decanted from the solid material in the flask
  3. additionIce was added to the flask
  4. dissolutionthe solid residue was dissolved in water
  5. extractionextracted with methylene chloride
  6. customThe phases were separated
  7. customhad been decanted from the reaction mixture
  8. washThis solution was washed in succession with a 5% aqueous solution of sodium hydroxide
  9. dry with materialAfter being dried over anhydrous magnesium sulfate
  10. filtrationfiltered
  11. customthe organic solution was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-16607fb47f1c4d9cba8fcdfc932b49f7
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05346881

反応ノート

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