Butyl bromide → 4-Bromo-1-butoxy-2-fluorobenzene

HRID 2068451

反応式

HRID 2068451 の反応式
[OH-].[Na+].[Br:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([F:11])[CH:5]=1.Br[CH2:13][CH2:14][CH2:15][CH3:16]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O>[Br:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:13][CH2:14][CH2:15][CH3:16])=[C:6]([F:11])[CH:5]=1

参加物

6

反応物 3

HCID 8002Butyl bromideHCID 14798Sodium HydroxideHCID 27249814-Bromo-2-fluorophenol

生成物 1

HCID 120674454-Bromo-1-butoxy-2-fluorobenzene収率 98.6%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

Sodium hydroxide (20.2 g) was added to a water (400 ml) solution of 4-bromo-2-fluorophenol (T-7) (76.4 g), bromobutane (65.8 g) and tetrabutylammonium bromide (TBAB) (6.44 g), and the mixture was heated with stirring at 80° C. for 6 hours under an atmosphere of nitrogen. After the completion of the reaction, the reaction mixture was extracted with heptane, and the organic layer was washed with water and brine, and then dried over anhydrous magnesium sulfate. The solution was concentrated under reduced pressure to leave a black oil. The oil was purified by distillation to give 4-bromo-1-butoxy-2-fluorobenzene (T-8) as a colorless oil (97.5 g) in 98% yield.

後処理

  1. temperaturethe mixture was heated
  2. customAfter the completion of the reaction
  3. extractionthe reaction mixture was extracted with heptane
  4. washthe organic layer was washed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe solution was concentrated under reduced pressure
  7. customto leave a black oil
  8. distillationThe oil was purified by distillation

出典と根拠

ORDレコード
ord-c6198ca4fe1649789b46752ecb41c113
出典データセット
uspto-grants-2012_10
特許番号
US08298632B2

関連ノート

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