Phosphorus oxychloride → Methyl 1-chloroisoquinoline-4-carboxylate

HRID 1826826Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1826826
O=[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]([O:14][CH3:15])=[O:13])=[CH:4][NH:3]1.O=P(Cl)(Cl)[Cl:18]>>[Cl:18][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]([O:14][CH3:15])=[O:13])=[CH:4][N:3]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 641184Methyl 1-Oxo-2H-Isoquinoline-4-Carboxylate

Produkt 1

HCID 3338790Methyl 1-chloroisoquinoline-4-carboxylate

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of the product from part 3 (12.5 g) in 50 ml of POCl3 is stirred at 100° C. for about two hours then cooled and concentrated under vacuum. The residue is dissolved in 300 ml of CHCl3, and the resulting solution is washed with aqueous NaHCO3 and water, dried over Na2SO4, filtered and then concentrated to give the title compound, m.p. 53–55° C.

Aufarbeitung

  1. temperaturethen cooled
  2. concentrationconcentrated under vacuum
  3. dissolutionThe residue is dissolved in 300 ml of CHCl3
  4. washthe resulting solution is washed with aqueous NaHCO3 and water
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-1d307f716c314e11a2b42032ec49d8b2
Quelldatensatz
uspto-grants-2006_05
Patentnummer
US07053093B2

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