2-Bromo-3,4-difluoro-1-nitrobenzene → HCID 66751543, 화합물

HRID 1962880노트

반응식

HRID 1962880 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 66751543HCID 66751543, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b742a7fc23ff493eb1986406ae538a3e
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415272B2

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