Hydrogen Bromide → 2-Bromo-2,4-dimethylpentan-3-one

HRID 411118

反応式

HRID 411118 の反応式
[CH3:1][CH:2]([C:4](=[O:8])[CH:5]([CH3:7])[CH3:6])[CH3:3].[Br:9]Br.Br>C(Cl)(Cl)Cl.C(=O)([O-])[O-].[Na+].[Na+]>[Br:9][C:2]([CH3:3])([C:4](=[O:8])[CH:5]([CH3:7])[CH3:6])[CH3:1]

参加物

6

反応物 3

HCID 260Hydrogen BromideHCID 112712,4-Dimethyl-3-pentanoneHCID 24408Bromine

生成物 1

HCID 2225752-Bromo-2,4-dimethylpentan-3-one収率 85.7%

試薬・触媒・溶媒 2

HCID 10340Sodium Carbonate触媒HCID 6212Chloroform溶媒

実験手順

2,4-dimethyl-3-pentanone (330 g, 2.89M) in chloroform (800 ml) was cooled in an ice water bath to 10° C. and bromine (462 g, 2.89M) was added slowly over 3 hours. After the addition, a slow stream of nitrogen was introduced to the mixture and HBr gas was slowly evolved from the flask. The nitrogen was left bubbling over a weekend to remove all of the HBr produced and then sodium carbonate (5 g) was added. The reaction mixture was then filtered through Celite and the chloroform removed using a rotary evaporator. Distillation of the crude product using a 1′ (2.54 cm) vigreux gave essentially pure 2-bromo-2,4-dimethyl-3-pentanone (478 g, 2.47M) b.pt. 50-52° C./10 mb (1000 Nm−2).

後処理

  1. additionAfter the addition
  2. waitThe nitrogen was left
  3. custombubbling over a weekend
  4. customto remove all of the HBr
  5. customproduced
  6. filtrationThe reaction mixture was then filtered through Celite
  7. customthe chloroform removed
  8. customa rotary evaporator
  9. distillationDistillation of the crude product

出典と根拠

ORDレコード
ord-9814e21addcb449e80b9977d407c4ae5
出典データセット
uspto-grants-2003_05
特許番号
US06559118B1

関連ノート

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