Pyrrolidine → Dimethyl 3,4-Dihydro-2,2-dimethyl-4-oxo-2H-1-benzopyran-6,7-dicarboxylate

HRID 36873Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 36873
[C:1]([C:4]1[CH:5]=[C:6]([C:15]([O:17][CH3:18])=[O:16])[C:7](=[CH:12][C:13]=1[OH:14])[C:8]([O:10][CH3:11])=[O:9])(=[O:3])[CH3:2].N1C[CH2:22][CH2:21][CH2:20]1>CC(C)=O>[CH3:20][C:21]1([CH3:22])[CH2:2][C:1](=[O:3])[C:4]2[CH:5]=[C:6]([C:15]([O:17][CH3:18])=[O:16])[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:12][C:13]=2[O:14]1

Komponenten

4

Edukt 2

HCID 31268PyrrolidineHCID 13227611Dimethyl 4-acetyl-5-hydroxyphthalate

Produkt 1

HCID 19936389Dimethyl 3,4-Dihydro-2,2-dimethyl-4-oxo-2H-1-benzopyran-6,7-dicarboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

In 100 ml of acetone was dissolved 4.2 g of dimethyl 4-acetyl-5-hydroxyphthalate synthesized in accordance with the process of Bulletin of the Chemical Society of Japan, Vol. 57, p. 3221 (1984). To the solution were added 1.0 ml of pyrrolidine and a small amount of Molecular Sieve (3A), followed by stirring at room temperature for 3 days. Any insoluble material was removed by filtration, and the solvent was removed by distillation under reduced pressure. The residue was purified by silica gel column chromatography to obtain 4.6 g (86.3%) of a yellow oily substance.

Aufarbeitung

  1. customsynthesized in accordance with the process of Bulletin of the Chemical Society of Japan, Vol. 57, p
  2. customAny insoluble material was removed by filtration
  3. customthe solvent was removed by distillation under reduced pressure
  4. customThe residue was purified by silica gel column chromatography
  5. customto obtain 4.6 g (86.3%) of a yellow oily substance

Quellen und Nachweise

ORD-Eintrag
ord-6f7e69cbea9b4ca2a006d71718374361
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05418232

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