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Methyl iodide → 1-Chloro-5-fluoro-2-methoxy-4-nitrobenzene

HRID 846505
ノート
印刷プレビュー

反応式

HRID 846505 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[OH:12].[C:13](=O)([O-])[O-].[K+].[K+].IC>CC(C)=O.C(OCC)C>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[O:12][CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 158655Phenol, 2-chloro-4-fluoro-5-nitro-

生成物 1

HCID 27792951-Chloro-5-fluoro-2-methoxy-4-nitrobenzene収率 76.4%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 3283Diethyl Ether溶媒

実験手順

To a stirred solution of 8.0 g (0.042 mole) of 2-chloro-4-fluoro-5-nitrophenol in 200 mL of acetone was added 6.09 g (0.0435 mole) of potassium carbonate. The mixture was heated at reflux temperature for 15 minutes, and 8.9 g (0.063 mole) of iodomethane was added. The resultant mixture was heated at reflux temperature for 5 hours, then stirred at room temperature for approximately 18 hours. The mixture was filtered and the filtrate evaporated under reduced pressure to leave a residue. The residue was dissolved in diethyl ether, filtered, and the filtrate washed with a saturated sodium chloride solution. The ether solution was dried over anhydrous sodium sulfate, filtered, and the filtrate evaporated to yield 6.6 g of 1-chloro-5-fluoro-2-methoxy-4-nitrobenzene as a solid, 63°-65° C.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux temperature for 15 minutes
  3. temperatureat reflux temperature for 5 hours
  4. filtrationThe mixture was filtered
  5. customthe filtrate evaporated under reduced pressure
  6. customto leave a residue
  7. filtrationfiltered
  8. washthe filtrate washed with a saturated sodium chloride solution
  9. dry with materialThe ether solution was dried over anhydrous sodium sulfate
  10. filtrationfiltered
  11. customthe filtrate evaporated

出典と根拠

ORDレコード
ord-4256073ea57c4139b0eefbdf6d0451b0
出典データセット
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05136868

反応ノート

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