3-Bromo-3-methyl-2-butanone → 2-Methyl-3-oxobutan-2-yl thiocyanate

HRID 544380Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 544380
Br[C:2]([CH3:7])([CH3:6])[C:3](=[O:5])[CH3:4].[C:8]([S-:10])#[N:9].[K+]>CC(C)=O>[CH3:6][C:2]([S:10][C:8]#[N:9])([CH3:7])[C:3](=[O:5])[CH3:4]

Komponenten

4

Edukt 2

HCID 3449113-Bromo-3-methyl-2-butanoneHCID 516872Potassium thiocyanate

Produkt 1

HCID 141951652-Methyl-3-oxobutan-2-yl thiocyanate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

16.5 g (0.1 mol) of 3-bromo-3-methyl-2-butanone and 11.6 g (0.12 mol) of potassium rhodanide in 150 ml of anhydrous acetone are heated at reflux for about 11/2 hours. After cooling, the separated potassium bromide is filtered off under suction and backwashed with a small amount of acetone, and the filtrate is evaporated to dryness at 50° C. under reduced pressure. The residue is dissolved in 200 ml of diethyl ether and the solution is washed three times with 100 ml of water each time, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure.The crude product is fractionated on a short Vigreux column to yield 3-methyl-3-thiocyanato-2-butanone, b.p. 52° C./0.04 mmHg.

Aufarbeitung

  1. temperatureat reflux for about 11/2 hours
  2. temperatureAfter cooling
  3. filtrationthe separated potassium bromide is filtered off under suction
  4. customthe filtrate is evaporated to dryness at 50° C. under reduced pressure
  5. dissolutionThe residue is dissolved in 200 ml of diethyl ether
  6. washthe solution is washed three times with 100 ml of water each time
  7. dry with materialdried over anhydrous sodium sulfate
  8. customevaporated to dryness under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7700561de3e445e3a587857853b19068
Quelldatensatz
uspto-grants-1984_05
Patentnummer
US04450157

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