Methylamine → HCID 83702359, Verbindung

HRID 1055661Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1055661
[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13](Cl)[N:14]=1)[C:8]([O:10]C)=[O:9])([CH3:4])([CH3:3])[CH3:2].[CH3:16][NH2:17]>>[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([NH:17][CH3:16])[N:14]=1)[C:8]([OH:10])=[O:9])([CH3:4])([CH3:3])[CH3:2]

Komponenten

3

Edukt 2

HCID 6329MethylamineHCID 86690963Methyl 2-chloro-6-(1,1-dimethylethyl)-4-pyridinecarboxylate

Produkt 1

HCID 83702359HCID 83702359, Verbindung

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

1.0 g (4.39 mmol) of methyl 2-tert-butyl-6-chloroisonicotinate [lit.: O. Isler et al., Helvetica Chimica Acta 1955, 38 (4), 1033-1046] and 3.8 ml (43.9 mmol) of a 40% strength aqueous methylamine solution were heated in a microwave oven (Biotage Initiator, with Dynamic Field Tuning) at 160° C. for 6 h. After cooling, the volatile components were removed on a rotary evaporator. The residue was taken up in 4 ml of semiconcentrated hydrochloric acid and once more heated in the microwave at 130° C. for 1 h. The product was then isolated directly by preparative HPLC (Method 12). Evaporation of the product fractions and drying of the residue under high vacuum gave 180 mg (92% pure, 18% of theory) of the title compound.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe volatile components were removed on a rotary evaporator
  3. customThe product was then isolated directly by preparative HPLC (Method 12)
  4. customEvaporation of the product fractions
  5. customdrying of the residue under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-82cd0cbe09a344a2bab0fa75633040ca
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09394309B2

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