Bromine → 2-Bromo-4-n-hexyl-1-methoxybenzene

HRID 1721432

反応式

HRID 1721432 の反応式
[CH2:1]([C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[Br:15]Br.S([O-])([O-])=O.[Na+].[Na+]>CO>[Br:15][C:11]1[CH:12]=[C:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[CH:8]=[CH:9][C:10]=1[O:13][CH3:14]

参加物

5

反応物 3

HCID 24408Bromine2 回HCID 24437Sodium SulfiteHCID 5785994-Hexylanisole

生成物 1

HCID 224149182-Bromo-4-n-hexyl-1-methoxybenzene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

26.4 g (0.137 mol) of 4-n-hexyl-1-methoxybenzene was dissolved in 200 ml of methanol. 26.4 g (0.156 mol) of bromine was added while stirring under cooling with ice. The mixture was stirred for 2 hours, while raising the temperature to room temperature. Sodium sulfite was added to the reaction mixture to decompose an excess amount of bromine, whereupon the mixture was extracted with chloroform-water. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue obtained was purified by column chromatography (silica gel, 20:1 mixture of n-hexane and ethyl acetate) to obtain 35.18 g (yield, 95.8%) of a colorless oil of the title compound.

後処理

  1. temperatureunder cooling with ice
  2. stirringThe mixture was stirred for 2 hours
  3. extractionwhereupon the mixture was extracted with chloroform-water
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue obtained
  8. customwas purified by column chromatography (silica gel, 20:1 mixture of n-hexane and ethyl acetate)
  9. customto obtain

出典と根拠

ORDレコード
ord-d9c6b350df924772831331b0c086fc2a
出典データセット
uspto-grants-1996_04
特許番号
US05510366

関連ノート

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