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

HRID 411118

반응식

HRID 411118 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 2225752-Bromo-2,4-dimethylpentan-3-one수율 85.7%

시약·촉매·용매 2

HCID 10340Sodium Carbonate촉매HCID 6212Chloroform용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9814e21addcb449e80b9977d407c4ae5
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559118B1

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