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Dimethylformamide → Benzyl 5-formyl-1H-pyrrole-2-carboxylate

HRID 2375795
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2375795
CN([CH:4]=[O:5])C.O=P(Cl)(Cl)Cl.[CH2:11]([O:18][C:19]([C:21]1[NH:22][CH:23]=[CH:24][CH:25]=1)=[O:20])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[C:26]([O-])(=[O:28])C.[Na+]>C(Cl)Cl.O>[CH2:11]([O:18][C:19]([C:21]1[NH:22][C:23]([CH:4]=[O:5])=[CH:24][CH:25]=1)=[O:20])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1.[CH2:11]([O:18][C:19]([C:21]1[NH:22][CH:23]=[C:24]([CH:26]=[O:28])[CH:25]=1)=[O:20])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1
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Komponenten

8

Edukt 4

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 517045Sodium AcetateHCID 8543774HCID 8543774, Verbindung

Produkt 2

HCID 71349636Benzyl 5-formyl-1H-pyrrole-2-carboxylateHCID 841032561H-Pyrrole-2-carboxylic acid, 4-formyl-, phenylmethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To DMF (5.93 g) was added POCl3 (12.45 g) dropwise at 0° C. The mixture was warmed to RT, diluted with DCM (40 mL) and cooled again to 0° C. A solution of 1H-pyrrole-2-carboxylic acid benzyl ester (15.00 g, prepared by adopting a procedure from J. Barry, G. Bram and A. Petit, Heterocycles 1985, 23, 875-880) in DCM (40 mL) was added dropwise at such a rate that the temperature of the reaction mixture did not rise above 0° C. The reaction was the heated to reflux for 30 min whereupon it was cooled to 10° C. A solution of sodium acetate (28g) in water (90 mL) was added carefully. After stirring for 15 min the two resulting phases were separated and the aqueous phase was washed with DCM (3×75 mL). The combined organic phases were washed with saturated Na2CO3 solution and brine, dried over MgSO4 and concentrated. The residue was purified by flash column chromatography on silica (ethyl acetate/heptanes 1:2) to provide 5-formyl-1H-pyrrole-2-carboxylic acid benzyl ester (8.0 g) and 4-formyl-1H-pyrrole-2-carboxylic acid benzyl ester (4.0 g).

Aufarbeitung

  1. temperaturecooled again to 0° C
  2. customdid not rise above 0° C
  3. temperatureheated
  4. temperatureto reflux for 30 min whereupon it
  5. temperaturewas cooled to 10° C
  6. customwere separated
  7. washthe aqueous phase was washed with DCM (3×75 mL)
  8. washThe combined organic phases were washed with saturated Na2CO3 solution and brine
  9. dry with materialdried over MgSO4
  10. concentrationconcentrated
  11. customThe residue was purified by flash column chromatography on silica (ethyl acetate/heptanes 1:2)

Quellen und Nachweise

ORD-Eintrag
ord-1f1278a2b66443fe9b0921c9123a3755
Quelldatensatz
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07465806B2

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