Potassium Nitrate → 2,5-Difluoro-1-methyl-3-nitrobenzene

HRID 1857418ノート

反応式

HRID 1857418 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH3:9].[N+:10]([O-])([O-:12])=[O:11].[K+]>OS(O)(=O)=O>[F:1][C:2]1[C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH3:9]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 679802,5-Difluorotoluene

生成物 1

HCID 552741502,5-Difluoro-1-methyl-3-nitrobenzene収率 91%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
28 °C

実験手順

To a stirred solution of 2,5-difluorotoluene (0.544 g, 4.25 mmol, Aldrich, used as received) in conc. H2SO4 (5.0 mL) at 0° C., KNO3 (0.430 g, 4.25 mmol) was added in one portion. The resulting pale yellow solution was warmed to 28° C. and stirred at that temperature overnight. It was then poured into ice (25 g) and extracted with ethyl acetate (40 mL). The extract was dried over Na2SO4 and evaporated to afford 0.555 g (91%) of the title compound as a light red oil; 1H NMR (CDCl3): 2.369 (d, 3H, J=1.8 Hz), 7.127 (dd, 1H, J1 =8.1 Hz, J2 =6.0 Hz), 7.734 (dd, 1H, J1 =8.4 Hz, J2 =6.3 Hz).

後処理

  1. extractionextracted with ethyl acetate (40 mL)
  2. dry with materialThe extract was dried over Na2SO4
  3. customevaporated

出典と根拠

ORDレコード
ord-7a81ac6fc04949d2aa53239f919dfa9e
出典データセット
uspto-grants-2000_11
特許番号
US06147075

反応ノート

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