Phosphorus tribromide → 1-(Bromomethyl)-2-fluoro-3-nitrobenzene

HRID 2061126ノート

反応式

HRID 2061126 の反応式
P(Br)(Br)[Br:2].[F:5][C:6]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:15]O>C(OCC)C>[Br:2][CH2:15][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]([N+:12]([O-:14])=[O:13])[C:6]=1[F:5]

参加物

4

反応物 2

HCID 24614Phosphorus tribromideHCID 29919768(2-Fluoro-3-nitrophenyl)methanol

生成物 1

HCID 591391511-(Bromomethyl)-2-fluoro-3-nitrobenzene収率 70%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of phosphorus tribromide (4.8 mL) in anhydrous diethylether (100 mL) was added at 0° C. to a solution of (2-fluoro-3-nitrophenyl)methanol (compound 2c-1) (7.52 g, 46.3 mmol) in anhydrous diethylether (130 mL), and the mixture was stirred at 30 minutes at 0° C. The reaction mixture was then poured into ice water and extracted with ethyl acetate. The organic extract was washed in series with saturated sodium hydrogen carbonate solution, water and saturated saline, and dried over magnesium sulfate. The title compound (7.10 g, 70%) was then obtained as a brown oil.

後処理

  1. extractionextracted with ethyl acetate
  2. extractionThe organic extract
  3. washwas washed in series with saturated sodium hydrogen carbonate solution, water and saturated saline
  4. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-556711d65878497e8c6f0bfef069f595
出典データセット
uspto-grants-2012_10
特許番号
US08278465B2

反応ノート

読み込み中…