Hydrochloric Acid → Texacromil

HRID 893988Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 893988
[OH:1][CH:2]([CH2:21][S:22][CH3:23])[CH2:3][O:4][C:5]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:6]=1[C:7](=[O:20])[CH:8]=[C:9]([C:15]([O:17]CC)=[O:16])[O:10]2.[OH-].[Na+].Cl>CC(C)=O>[OH:1][CH:2]([CH2:21][S:22][CH3:23])[CH2:3][O:4][C:5]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:6]=1[C:7](=[O:20])[CH:8]=[C:9]([C:15]([OH:17])=[O:16])[O:10]2

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12888660Ethyl 5-(2-hydroxy-3-methylthiopropoxy)chromone-2-carboxylate

Produkt 1

HCID 3086067TexacromilAusbeute 89,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of 3.4 g of ethyl 5-(2-hydroxy-3-methylthiopropoxy)chromone-2-carboxylate in 20 ml of acetone there is added 11 ml of N sodium hydroxide and the mixture is heated at 50° C. for 10 minutes. After evaporating the solvent under reduced pressure, 30 ml of water are added, the resulting mixture is extracted with diethyl ether, filtered on charcoal and the limpid solution thus obtained is acidified with hydrochloric acid. The product which precipitates is filtered, washed with water and dried. Thus, 2.8 g of 5-(2-hydroxy-3-methylthiopropoxy)chromone-2-carboxylic acid is obtained as dihydrate (CM 57202); m.p. 76°-79° C.

Aufarbeitung

  1. customAfter evaporating the solvent under reduced pressure, 30 ml of water
  2. additionare added
  3. extractionthe resulting mixture is extracted with diethyl ether
  4. filtrationfiltered on charcoal
  5. customthe limpid solution thus obtained
  6. customThe product which precipitates
  7. filtrationis filtered
  8. washwashed with water
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-df7d36e322714315860f889fb0aac1f0
Quelldatensatz
uspto-grants-1981_08
Patentnummer
US04282247

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