N-bromobutanimide → Benzene, 1,3-dibromo-2,4-dimethoxy-

HRID 470724

反応式

HRID 470724 の反応式
[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[CH:4][C:3]=1[O:10][CH3:11].[Br:12]N1C(=O)CCC1=O>C(#N)C>[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[C:4]([Br:12])[C:3]=1[O:10][CH3:11]

参加物

4

反応物 2

HCID 67184N-bromobutanimide2 回HCID 6122962-Bromo-1,3-dimethoxybenzene

生成物 1

HCID 11645053Benzene, 1,3-dibromo-2,4-dimethoxy-収率 95.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

17.9 g of 1-bromo-2,6-dimethoxybenzene and 200 mL of acetonitrile were placed in a flask, and the resulting mixture was cooled on ice. Then, 14.7 g of N-bromosuccinimide was added. Then, while heating the reaction solution to room temperature, stirring was conducted for 8 hours. 2.39 g of N-bromosuccinimide was further added, and stirring was conducted at room temperature for 7 hours. After completion of the stirring, the solvent was distilled off under reduced pressure. Residues were dissolved in dichloromethane, and washed sequentially with sodium thiosulfate and saturated saline. An organic phase was dried with magnesium sulfate and concentrated. Residues were purified by means of silica gel column chromatography, whereby 23.2 g (yield: 95%) of colorless oil of 1,3-bromo-2,6-dimethoxybenzene was obtained.

後処理

  1. temperaturethe resulting mixture was cooled on ice
  2. stirringstirring
  3. waitwas conducted at room temperature for 7 hours
  4. distillationAfter completion of the stirring, the solvent was distilled off under reduced pressure
  5. dissolutionResidues were dissolved in dichloromethane
  6. washwashed sequentially with sodium thiosulfate and saturated saline
  7. dry with materialAn organic phase was dried with magnesium sulfate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-67e35be1c97743f6a2c25e17dc1f599b
出典データセット
uspto-grants-2014_01
特許番号
US08629430B2

関連ノート

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