m-Chloroperbenzoic acid → Hydrochloric Acid

HRID 1074931Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1074931
Cl.[F:2][C:3]([F:19])([F:18])[C:4]1[CH:5]=[C:6]([S:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)[CH:7]=[CH:8][CH:9]=1.[Cl:20]C1C=C(C=CC=1)C(OO)=[O:25]>C(Cl)Cl>[F:19][C:3]([F:2])([F:18])[C:4]1[CH:5]=[C:6]([S:10]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)=[O:25])[CH:7]=[CH:8][CH:9]=1.[ClH:20]

Komponenten

5

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 129532902-({[3-(Trifluoromethyl)phenyl]sulfanyl}methyl)pyridine--hydrogen chloride (1/1)

Produkt 2

HCID 313Hydrochloric AcidAusbeute 419,3 %HCID 127602352-{[3-(Trifluoromethyl)benzene-1-sulfinyl]methyl}pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A stirred suspension of 2-(((3-trifluoromethylphenyl)thio)methylpyridine, hydrochloride (2.0 g) in methylene chloride (50 ml) at 0° C. was treated portionwise with m-chloroperoxybenzoic acid (1.5 g) over 1/2 hour. The mixture was allowed to warm to ambient temperature and the mixture was stirred a further 1/2 hour. The solution was washed with saturated Na2CO3 solution and water, dried (MgSO4) and evaporated. The residue was converted into the hydrochloride, in acetone with ethereal HCl solution, which was recrystallised from acetone-ether to give the title compound, hydrochloride (1.0 g) mp 135°-6° C. (Found: C,48.3; H,3.7; N,4.0 C13H10F3NOS.HCl requires C,48.4; H,3.45; N,4.35%).

Aufarbeitung

  1. washThe solution was washed with saturated Na2CO3 solution and water
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customwas recrystallised from acetone-ether

Quellen und Nachweise

ORD-Eintrag
ord-d05d22edf9d648a6a8262aa293f52237
Quelldatensatz
uspto-grants-1983_07
Patentnummer
US04394509

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