Methyl morpholine oxide → HCID 19611677, Verbindung

HRID 1602380Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1602380
C[N+]1([O-])CC[O:5]CC1.Br[CH2:10][C:11]1[C:16]2[CH:17]=[CH:18][O:19][C:15]=2[C:14]([Cl:20])=[CH:13][CH:12]=1>C(#N)C>[Cl:20][C:14]1[CH:13]=[CH:12][C:11]([CH:10]=[O:5])=[C:16]2[C:15]=1[O:19][CH:18]=[CH:17]2

Komponenten

4

Edukt 2

HCID 82029Methyl morpholine oxideHCID 19611696HCID 19611696, Verbindung

Produkt 1

HCID 19611677HCID 19611677, VerbindungAusbeute 73,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A solution of the N-methylmorpholine-N-oxide (37.64 g) in aoetonitrile (370 ml) containing 3 Å molecular sieves (36.6 g) was stirred at room temperature overnight and cooled in ice. A solution of 4-bromomethyl-7-chloro-benzofuran (39.44 g) in acetonitrile (90 ml) was added and the mixture stirred in at 0° C. for 4 h. The mixture was filtered and the filtrate evaporated to dryness. Water and ethyl acetate were added to the residue and the organic phase separated, dried (Na2SO4) and evaporated to give the title compound (21.3 g) as a pale yellow solid.

Aufarbeitung

  1. temperaturecooled in ice
  2. stirringthe mixture stirred in at 0° C. for 4 h
  3. filtrationThe mixture was filtered
  4. customthe filtrate evaporated to dryness
  5. additionWater and ethyl acetate were added to the residue
  6. customthe organic phase separated
  7. dry with materialdried (Na2SO4)
  8. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-e3b7f707ab4d4a74beb84622911d5f84
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05981572

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