Bromine → 1-Bromo-2,4-dimethoxy-5-nitrobenzene

HRID 844296

反応式

HRID 844296 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[N+:11]([O-:13])=[O:12].[Br:14]Br.S(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[Br:14][C:6]1[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]([O:2][CH3:1])=[CH:8][C:7]=1[O:9][CH3:10]

参加物

5

反応物 3

HCID 24408Bromine2 回HCID 786332,4-Dimethoxy-1-nitrobenzeneHCID 23665763Sodium Bisulfite

生成物 1

HCID 185436101-Bromo-2,4-dimethoxy-5-nitrobenzene

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒3 回

実験手順

To a solution of 2,4-dimethoxy-nitrobenzene (0.50 g) in chloroform (3 mL) is added dropwise a solution of bromine (0.23 g) in chloroform (1 mL) and the mixture is allowed to stir at room temperature for approximately 15 hours. Additional bromine (0.15 g) in chloroform (1 mL) is added and the reaction is stirred for an additional 4 hours. The mixture is then poured onto 5% aqueous sodium bisulfite and then extracted with chloroform. Pooled organic extracts are then washed successively with 5% aqueous sodium bisulfite then saturated sodium chloride, and then dried over anhydrous sodium sulfate. Removal of the solvent under reduced pressure and recrystallization of the residue from toluene provides the desired product as a yellow solid.

後処理

  1. stirringthe reaction is stirred for an additional 4 hours
  2. extractionextracted with chloroform
  3. washPooled organic extracts are then washed successively with 5% aqueous sodium bisulfite
  4. dry with materialsaturated sodium chloride, and then dried over anhydrous sodium sulfate
  5. customRemoval of the solvent
  6. customunder reduced pressure and recrystallization of the residue from toluene

出典と根拠

ORDレコード
ord-fac832a8573a4e2b99a8993e190f8d4d
出典データセット
uspto-grants-2002_04
特許番号
US06380243B1

関連ノート

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