Potassium Carbonate → 2-(1,3-Dioxolan-2-yl)-6-methylpyridine 1-oxide

HRID 1258580Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1258580
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH3:12])[N:7]=1.C1C=C(Cl)C=C(C(OO)=[O:21])C=1.C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH3:12])[N+:7]=1[O-:21]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 27343042-(1,3,-Dioxolan-2-yl)-6-methylpyridine

Produkt 1

HCID 671899662-(1,3-Dioxolan-2-yl)-6-methylpyridine 1-oxideAusbeute 84,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution 2-(1,3-dioxolan-2-yl)-6-methylpyridine (3.7 g, 15.67 mmol, 1 eq.) in 200 ml of DCM was added mCPBA (7.21 g, 31.35 mmol, 2 eq.) portionwise (exotherm 20° C.>26° C.). The reaction was stirred for 1 hr and 100 ml of 2M aqueous K2CO3 solution was added. The mixture was stirred for 15 mins and the organic layer was separated, washed with water (100 ml), dried over MgSO4 and evaporated to give 2-(1,3-dioxolan-2-yl)-6-methylpyridine 1-oxide (2.4 g, 80% yield) as a yellow liquid.

Aufarbeitung

  1. stirringThe mixture was stirred for 15 mins
  2. customthe organic layer was separated
  3. washwashed with water (100 ml)
  4. dry with materialdried over MgSO4
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-2bc57693ea5e458bb7b80e05fb4286e2
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08466176B2

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