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Methyl iodide → 1,5-Difluoro-3-methoxy-2-nitrobenzene

HRID 871856
ノート
印刷プレビュー

反応式

HRID 871856 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4](F)[C:3]=1[N+:10]([O-:12])=[O:11].[C:13]([O-])([O-])=[O:14].[K+].[K+].CI>CC(C)=O>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4]([O:14][CH3:13])[C:3]=1[N+:10]([O-:12])=[O:11]
参加物反応条件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 6328Methyl iodideHCID 11430Potassium CarbonateHCID 675671,3,5-Trifluoro-2-nitrobenzene

生成物 1

HCID 103301291,5-Difluoro-3-methoxy-2-nitrobenzene収率 95%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
50 °C

実験手順

To a solution of 2.45 g (14.0 mmol) of 1,3,5-trifluoro-2-nitrobenzene in acetone are successively added 2.9 g (21.0 mmol) of K2CO3 powder and 3.5 mL (56.0 mmol) of methyl iodide. The reaction mixture is heated at 50°C. for 2 hours and then filtered and evaporated to dryness. The residue is taken up in ethyl acetate and washed with water and with saturated aqueous NaCl solution. The organic phase is dried over Na2SO4, filtered and concentrated under vacuum. 2.52 g of the expected product are recovered in the form of a yellow solid, which is used as obtained in the following step. Yield=95%.

後処理

  1. filtrationfiltered
  2. customevaporated to dryness
  3. washwashed with water and with saturated aqueous NaCl solution
  4. dry with materialThe organic phase is dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. custom2.52 g of the expected product are recovered in the form of a yellow solid, which
  8. customas obtained in the following step

出典と根拠

ORDレコード
ord-9bc0aa9bb43c41db873da6befeb00ae8
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08975250B2

反応ノート

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