Potassium Nitrate → 5-Bromo-6-fluoro-8-nitroquinaldine

HRID 434667

反応式

HRID 434667 の反応式
[N+:1]([O-:4])([O-])=[O:2].[K+].[Br:6][C:7]1[C:16]([F:17])=[CH:15][CH:14]=[C:13]2[C:8]=1[CH:9]=[CH:10][C:11]([CH3:18])=[N:12]2>S(=O)(=O)(O)O.ClCCl>[Br:6][C:7]1[C:16]([F:17])=[CH:15][C:14]([N+:1]([O-:4])=[O:2])=[C:13]2[C:8]=1[CH:9]=[CH:10][C:11]([CH3:18])=[N:12]2

参加物

5

反応物 2

HCID 24434Potassium NitrateHCID 130353135-Bromo-6-fluoro-2-methylquinoline

生成物 1

HCID 131919625-Bromo-6-fluoro-8-nitroquinaldine収率 91.8%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

A solution of 11.5 g of potassium nitrate in 30 ml of concentrated sulfuric acid was added to 21.0 g of 5-bromo-6-fluoroquinaldine in 117 ml of concentrated sulfuric acid dropwise at -5° C. After stirring at room temperature for 5 hours, the reaction mixture was poured into 2 l of ice water to precipitate solids which were then collected by filtration. The filtrate was rendered alkaline to form a small amount of solids, which together with the former solids were dissolved in dichloromethane. After the solution was dried over sodium sulfate the solvent was distilled off. Recrystallization of the residue from isopropanol gave 22.9 g of 5-bromo-6-fluoro-8-nitroquinaldine. m.p. 135°-137° C.

後処理

  1. customto precipitate solids which
  2. filtrationwere then collected by filtration
  3. customto form a small amount of solids, which together with the former solids
  4. dry with materialAfter the solution was dried over sodium sulfate the solvent
  5. distillationwas distilled off
  6. customRecrystallization of the residue from isopropanol

出典と根拠

ORDレコード
ord-3ce4858b3b4c477693aa3864b68984a6
出典データセット
uspto-grants-1983_08
特許番号
US04399134

関連ノート

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