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

HRID 470724

반응식

HRID 470724 반응식
[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]

참가 물질

4

반응물 2

HCID 67184N-bromobutanimide2회HCID 6122962-Bromo-1,3-dimethoxybenzene

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-67e35be1c97743f6a2c25e17dc1f599b
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629430B2

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