Methyl iodide → HCID 54010899, Verbindung

HRID 2165217Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2165217
[CH3:1]I.[Mg].C[C:5]1[C:12]([F:13])=[C:11]([F:14])[C:8]([CH:9]=[O:10])=[C:7]([F:15])[C:6]=1[F:16].[Cl-].[NH4+]>C(OCC)C>[CH3:1][CH:9]([OH:10])[C:8]1[C:7]([F:15])=[C:6]([F:16])[CH:5]=[C:12]([F:13])[C:11]=1[F:14]

Komponenten

6

Edukt 4

HCID 6328Methyl iodideHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 132680124-Methyl-2,3,5,6-tetrafluoro-benzaldehyde

Produkt 1

HCID 54010899HCID 54010899, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

3 2 ml of methyl iodide were introduced over the course of 30 minutes into a suspension of 1 g of magnesium and 30 ml of ethyl ether and the mixture was stirred for 30 minutes. The mixture was cooled to 0° C. and 4 g of 4-methyl-2,3,5,6-tetra fluorobenzaldehyde and 100 ml of ethyl ether were introduced over the course of 30 minutes. The reaction mixture was stirred for 1 hour at 0° C. and was poured into 150 ml of a saturated aqueous ammonium chloride solution. Extraction was carried out with ether and the ethereal phases were dried and evaporated to dryness under reduced pressure. The crude product was chromatographed on silica and eluted with a hexane:isopropyl ether (8:2) mixture to obtain 3.85 g of the product with a Rf=0.10.

Aufarbeitung

  1. stirringThe reaction mixture was stirred for 1 hour at 0° C.
  2. extractionExtraction
  3. customthe ethereal phases were dried
  4. customevaporated to dryness under reduced pressure
  5. customThe crude product was chromatographed on silica
  6. washeluted with a hexane:isopropyl ether (8:2) mixture

Quellen und Nachweise

ORD-Eintrag
ord-4b24874aac494aa9a688b1d0ad96eb3c
Quelldatensatz
uspto-grants-1990_07
Patentnummer
US04939172

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