Bromine → HCID 23465925, compound

HRID 443843Notes

Reaction equation

HRID 443843 reaction equation
[CH3:1][C:2]([CH3:14])([CH3:13])[C:3](=[O:12])[CH2:4][CH2:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1.[Br:15]Br>Br>[Br:15][CH:4]([C:3](=[O:12])[C:2]([CH3:14])([CH3:13])[CH3:1])[CH2:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1

Participants

4

Reactant 2

HCID 24408BromineHCID 4547109HCID 4547109, compound

Product 1

HCID 23465925HCID 23465925, compoundYield 100.9%

Reagents, catalysts & solvents 1

HCID 260Hydrogen BromideSolvent

Procedure

320.5 g (1.676 mol) of 4,4-dimethyl-1-pyridin-3-yl-pentan-3-one were dissolved in 320 ml of aqueous 48% strength hydrobromic acid, and 267.8 g (85.3 ml; 1.65 mol) of bromine were added dropwise at 80° to 95° C. in the course of 2 hours. When the addition had ended, the solution was cooled and concentrated. The solid which remained was comminuted well, stirred with about 1.5 liters of ethanol, filtered off, washed with ethanol and dried. 450 g (78% of theory) of 2-bromo-4,4-dimethyl-1-pyridin-3-yl-pentan-3-one of melting point 163°-64° C. were obtained. ##STR119##

Workup

  1. additionwere added dropwise at 80° to 95° C. in the course of 2 hours
  2. additionWhen the addition
  3. temperaturethe solution was cooled
  4. concentrationconcentrated
  5. customThe solid which remained was comminuted well
  6. filtrationfiltered off
  7. washwashed with ethanol
  8. customdried

Sources & evidence

ORD record
ord-20a68870072b497ab42549030f488934
Source dataset
uspto-grants-1981_04
Patent number
US04262000

Reaction notes

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