Potassium Nitrate → 1-Chloro-4-fluoro-2-methyl-5-nitrobenzene

HRID 1068657ノート

反応式

HRID 1068657 の反応式
[Cl: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>[Cl:1][C:2]1[CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]([F:8])=[CH:4][C:3]=1[CH3:9]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 1184752-Chloro-5-fluorotoluene

生成物 1

HCID 103524921-Chloro-4-fluoro-2-methyl-5-nitrobenzene

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

To a stirred solution of 2-chloro-5-fluorotoluene (10.356 g, 71.628 mmol, Lancaster, used as received) in conc. H2SO4 (70 mL) at 0° C., KNO3 (7.252 g, 71.72 mmol) was added in four equal portions. The resulting pale yellow solution was allowed to warm to room temperature and was stirred overnight at room temperature. It was then poured into ice water (350 g) and extracted with ether (3×100 mL). Ether was dried over anhydrous Na2SO4, removed under vacuum, and the resulting oil was dried further under vacuum to afford 12.277 g (90%). of the title compound as an oil, which was used as such for the next reaction; 1H NMR (CDCl3); δ 2.459 (s, 2H), 7.193 (d, 1H, J1=11.1 Hz), 8.083 (d, 1H, J1=6.6 Hz).

後処理

  1. extractionextracted with ether (3×100 mL)
  2. dry with materialEther was dried over anhydrous Na2SO4
  3. customremoved under vacuum
  4. customthe resulting oil was dried further under vacuum
  5. customto afford 12.277 g (90%)

出典と根拠

ORDレコード
ord-370e3688c4484388827b3cd351071cf3
出典データセット
uspto-grants-2001_06
特許番号
US06251903B1

反応ノート

読み込み中…