m-Chloroperbenzoic acid → HCID 21873713, Verbindung

HRID 1913433Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1913433
[CH3:1][C:2]1[N:7]=[C:6]2[O:8][CH2:9][CH2:10][O:11][C:5]2=[CH:4][CH:3]=1.C1C=C(Cl)C=C(C(OO)=[O:20])C=1>C(Cl)Cl>[CH3:1][C:2]1[N+:7]([O-:20])=[C:6]2[O:8][CH2:9][CH2:10][O:11][C:5]2=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 156332996-Methyl-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine

Produkt 1

HCID 21873713HCID 21873713, VerbindungAusbeute 74,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a 0° C. solution of 6-methyl-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine (19 g, 0.12 mol) in anhydrous CH2Cl2 (250 mL) was added m-CPBA (32 g, 0.15 mol) portionwise. The mixture was stirred at room temperature overnight. The solvent was removed in vacuo and the residue was purified via column chromatography (silica gel, EtOAc/petroleum ether 1:1) to yield 6-methyl-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine 5-oxide (15.0 g, 72%) as a white solid.

Aufarbeitung

  1. customThe solvent was removed in vacuo
  2. customthe residue was purified via column chromatography (silica gel, EtOAc/petroleum ether 1:1)

Quellen und Nachweise

ORD-Eintrag
ord-c719cb5409ab47ddaa7edcf1c5aa1156
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08609680B2

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