Methanol → 1-Bromo-2-fluoro-5-methoxy-4-nitrobenzene

HRID 419448

反応式

HRID 419448 の反応式
[Br:1][C:2]1[CH:7]=[C:6](F)[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[F:12].[CH3:13][O-:14].[Na+].CO>C(Cl)Cl>[CH3:13][O:14][C:6]1[CH:7]=[C:2]([Br:1])[C:3]([F:12])=[CH:4][C:5]=1[N+:9]([O-:11])=[O:10]

参加物

5

反応物 3

HCID 887MethanolHCID 27362864-Bromo-2,5-difluoronitrobenzeneHCID 10942334Sodium Methoxide

生成物 1

HCID 223473121-Bromo-2-fluoro-5-methoxy-4-nitrobenzene収率 95.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
60 °C

実験手順

To 1-bromo-2,5-difluoro-4-nitrobenzene (5.0 g, 21 mmol) was added 0.5 N sodium methoxide (50 mL, 25 mmol). The mixture was stirred at 60° C. for 1 h. The MeOH was rotovaped down. The crude product was dissolved in DCM (100 mL), washed with H2O, dried (Na2SO4), filtered, and rotovaped down to give the title compound of step A (5 g, 20 mmol, 95%) as a yellow solid. 1H NMR (400 MHz, CDCl3) δ ppm 7.69 (s, 1H), 7.28 (s, 1H), 3.95 (s, 3H).

後処理

  1. washwashed with H2O
  2. dry with materialdried (Na2SO4)
  3. filtrationfiltered

出典と根拠

ORDレコード
ord-f3a7673b827643669d7dc4972db4a14c
出典データセット
uspto-grants-2012_01
特許番号
US08093239B2

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