Benzoyl Peroxide → HCID 22615271, Verbindung

HRID 842708

Reaktionsgleichung

Reaktionsgleichung von HRID 842708
C1C(=O)N([Cl:8])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.[Cl:27][C:28]1[C:33]([C:34]#[N:35])=[CH:32][CH:31]=[C:30]([CH3:36])[N:29]=1>C1C=CC=CC=1>[Cl:27][C:28]1[C:33]([C:34]#[N:35])=[CH:32][CH:31]=[C:30]([CH2:36][Cl:8])[N:29]=1

Komponenten

5

Versuchsvorschrift

NCS (1.44 g, 10.8 mmol) and benzoyl peroxide (238 mg, 0.98 mmol) were added to a stirred solution of 2-chloro-3-cyano-6-methyl-pyridine (750 mg, 4.92 mmol) in benzene (35 mL) and the mixture was heated to reflux. After 4 h, the mixture was cooled and filtered. The filtrate was diluted with ethyl acetate and was washed with sodium metabisulfite solution, water and brine, dried (Na2SO4) and evaporated in vacuo. The residue was purified by chromatography on silica (chloroform) to give the title compound:

Aufarbeitung

  1. temperaturethe mixture was heated to reflux
  2. temperaturethe mixture was cooled
  3. filtrationfiltered
  4. additionThe filtrate was diluted with ethyl acetate
  5. washwas washed with sodium metabisulfite solution, water and brine
  6. dry with materialdried (Na2SO4)
  7. customevaporated in vacuo
  8. customThe residue was purified by chromatography on silica (chloroform)

Quellen und Nachweise

ORD-Eintrag
ord-770e2c5221a6477481db72971c6ebf26
Quelldatensatz
uspto-grants-2002_04
Patentnummer
US06376499B1

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