2-Bromo-3,4-difluoro-1-nitrobenzene → HCID 66751543、化合物

HRID 1962880ノート

反応式

HRID 1962880 の反応式
[CH3:1][O-:2].[Na+].[Br:4][C:5]1[C:10]([F:11])=[C:9](F)[CH:8]=[CH:7][C:6]=1[N+:13]([O-:15])=[O:14]>CS(C)=O>[Br:4][C:5]1[C:10]([F:11])=[C:9]([O:2][CH3:1])[CH:8]=[CH:7][C:6]=1[N+:13]([O-:15])=[O:14]

参加物

4

反応物 2

HCID 5745892-Bromo-3,4-difluoro-1-nitrobenzeneHCID 10942334Sodium Methoxide

生成物 1

HCID 66751543HCID 66751543、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

NaOMe (9.5 g) was added portion wise to a solution of 2-bromo-3,4-difluoro-1-nitro-benzene (21.0 g) dissolved in DMSO (250 ml) at room temperature under nitrogen atmosphere. The mixture was stirred for 3 hrs and then poured onto water and extracted with ethyl acetate. The organic phase was extracted with water and brine, dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude product, 2-bromo-3-fluoro-4-methoxy-1-nitro-benzene was used as such in Step 2 described below. 1H NMR (CDCl3) δ ppm: 7.85 (1H, dd); 6.99 (1H, dd); 3.99 (3H, s).

後処理

  1. additionpoured onto water
  2. extractionextracted with ethyl acetate
  3. extractionThe organic phase was extracted with water and brine
  4. dry with materialdried over anhydrous sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b742a7fc23ff493eb1986406ae538a3e
出典データセット
uspto-grants-2013_04
特許番号
US08415272B2

反応ノート

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