Diethyl methylmalonate → HCID 58280423, Verbindung

HRID 1506877Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1506877
[F:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([F:9])[C:7]=1F.[CH3:13][CH:14]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:15]([O:17][CH2:18][CH3:19])=[O:16].[OH-].[Na+]>CN(C=O)C>[F:9][C:6]1[CH:5]=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=[C:2]([F:1])[C:7]=1[C:14]([CH3:13])([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:20]([O:22][CH2:23][CH3:24])=[O:21]

Komponenten

5

Edukt 3

HCID 11857Diethyl methylmalonateHCID 14798Sodium HydroxideHCID 27827931,2,3-Trifluoro-5-nitrobenzene

Produkt 1

HCID 58280423HCID 58280423, VerbindungAusbeute 76,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of commercially available 3,4,5-trifluoro-nitrobenzene (25b) (5.0 mL, 42.8 mmol), diethyl methylmalonate (6.1 mL, 35.7 mmol), and sodium hydroxide (1.54 g, 38.5 mmol) in DMF (55 mL) was allowed to react in the same manner as in (a) in Production Example 1. The crude product was subjected to silica gel column chromatography and elution with an n-hexane/ethyl acetate (10:1) solution to give 9.1 g (63%) of compound (26b) of interest as clear brown oil.

Aufarbeitung

  1. washThe crude product was subjected to silica gel column chromatography and elution with an n-hexane/ethyl acetate (10:1) solution

Quellen und Nachweise

ORD-Eintrag
ord-14129075846a4110b3e616f7e63c679b
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09221786B2

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