Hydrochloric Acid → HCID 20304505, Verbindung

HRID 1732737Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1732737
[CH3:1][C:2]1[C:3](=[O:24])[C:4]2[CH:20]=[C:19]3[C:14]([CH2:15][CH2:16][CH2:17][CH2:18]3)=[C:13]([CH2:21][CH2:22][CH3:23])[C:5]=2[O:6][C:7]=1[C:8]([O:10]CC)=[O:9].Cl>C(O)(=O)C>[CH3:1][C:2]1[C:3](=[O:24])[C:4]2[CH:20]=[C:19]3[C:14]([CH2:15][CH2:16][CH2:17][CH2:18]3)=[C:13]([CH2:21][CH2:22][CH3:23])[C:5]=2[O:6][C:7]=1[C:8]([OH:10])=[O:9]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 20304565HCID 20304565, Verbindung

Produkt 1

HCID 20304505HCID 20304505, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A mixture of the product of step (f) (16.2 g), glacial acetic acid (80 ml) and 5 N hydrochloric acid (20 ml) was heated and stirred on a steam bath overnight, and then evaporated. The residue was extracted with aqueous sodium bicarbonate and the extract was filtered and then acidified. Precipitated material was isolated by decantation and was triturated with water, dried, then triturated with an ether/petroleum ether (40°-60°) mixture. There remained as an insoluble off-white solid, 6,7,8,9-tetrahydro-3-methyl-4-oxo-10-propyl-4H-naphtho[2,3-b]pyran-2-carboxylic acid, (3.5 g), m.p 162°-4°.

Aufarbeitung

  1. temperaturewas heated
  2. customevaporated
  3. extractionThe residue was extracted with aqueous sodium bicarbonate
  4. filtrationthe extract was filtered
  5. customPrecipitated material was isolated by decantation
  6. customwas triturated with water
  7. customdried
  8. customtriturated with an ether/petroleum ether (40°-60°) mixture
  9. customremained as an insoluble off-white solid, 6,7,8,9-tetrahydro-3-methyl-4-oxo-10-propyl-4H-naphtho[2,3-b]pyran-2-carboxylic acid, (3.5 g), m.p 162°-4°

Quellen und Nachweise

ORD-Eintrag
ord-d5a167f06cdf446786503983b9b3e6f5
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04238606

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