Bromine → 3-Bromo-2,6-diethyl-benzaldehyde

HRID 254498ノート

反応式

HRID 254498 の反応式
[Cl-].[Cl-].[Cl-].[Al+3].[CH2:5]([C:7]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH3:16])[C:8]=1[CH:9]=[O:10])[CH3:6].[Br:17]Br>ClCCl>[Br:17][C:14]1[C:7]([CH2:5][CH3:6])=[C:8]([C:11]([CH2:15][CH3:16])=[CH:12][CH:13]=1)[CH:9]=[O:10]

参加物

5

反応物 3

HCID 24408BromineHCID 6451240Aluminum(III) ChlorideHCID 131847782,6-Diethylbenzaldehyde

生成物 1

HCID 589518323-Bromo-2,6-diethyl-benzaldehyde

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
40 °C

実験手順

To a solution of 8.01 g (60 mmol) aluminum trichloride in 10 ml dichloromethane were added at ambient temperature drop-wise 5.52 g (34 mmol) 2,6-diethyl-benzaldehyde (Example 1 c)); exothermic reaction. To the resulting dark red solution was added slowly drop-wise a solution of 5.5 g (34 mmol) bromine in 7 ml dichloromethane; strong exothermic reaction. Then the mixture was heated to 40° C. for 3 hours. The reaction mixture was cooled to ambient temperature and poured onto ice. The organic phase was separated and the aqueous solution extracted with dichloromethane, the combined extracts washed with 2N HCl solution, saturated sodium bicarbonate solution and brine, dried over MgSO4, filtered and evaporated: 7.0 g 3-bromo-2,6-diethyl-benzaldehyde of 90% purity (HPLC) that did not require further purification.

後処理

  1. customexothermic reaction
  2. customstrong exothermic reaction
  3. temperatureThe reaction mixture was cooled to ambient temperature
  4. additionpoured onto ice
  5. customThe organic phase was separated
  6. extractionthe aqueous solution extracted with dichloromethane
  7. washthe combined extracts washed with 2N HCl solution, saturated sodium bicarbonate solution and brine
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customevaporated
  11. custompurification

出典と根拠

ORDレコード
ord-50f79f7183b447bd98d6dc2a147c6760
出典データセット
uspto-grants-2011_01
特許番号
US07875645B2

反応ノート

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