Potassium Nitrate → 1-Bromo-5-fluoro-4-nitro-2-(trifluoromethyl)benzene

HRID 2064157ノート

反応式

HRID 2064157 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([F:12])([F:11])[F:10].[N+:13]([O-])([O-:15])=[O:14].[K+]>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N+:13]([O-:15])=[O:14])=[CH:4][C:3]=1[C:9]([F:12])([F:10])[F:11]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 27349092-Bromo-4-fluorobenzotrifluoride

生成物 1

HCID 594197851-Bromo-5-fluoro-4-nitro-2-(trifluoromethyl)benzene収率 101.6%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
0 °C

実験手順

A stirred solution of 2-bromo-4-fluorobenzotrifluoride (1.0 g, 4.1 mmole) in concentrated sulphuric acid (10 ml) at 0° C. was treated portionwise with KNO3 (0.46 g, 4.6 mmole) and maintained at 0° C. for 0.5 hr before warming to room temp. over 2 hr. The mixture was added to well stirred ice/water (100 ml) and then extracted with ethyl acetate. The extract was dried and concentrated under vacuum to afford the title compound as a yellow solid (1.2 g, 100%). 1H NMR (400 MHz, CDCl3) δ: 7.75 (1H, d), 8.45 (1H, d).

後処理

  1. temperaturebefore warming to room temp. over 2 hr
  2. extractionextracted with ethyl acetate
  3. customThe extract was dried
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-536b3c8d1aec427ca9e4004801257f18
出典データセット
uspto-grants-2012_10
特許番号
US08288412B2

反応ノート

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