Hydrochloric Acid → 2-(3,4-Dichlorobenzyl)-5-methyl-4-oxo-3,4-dihydrothieno(2,3-d)pyrimidine-6-carboxylic acid

HRID 403455Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 403455
[Na+].[Cl:2][C:3]1[CH:4]=[C:5]([CH:21]=[CH:22][C:23]=1[Cl:24])[CH2:6][C:7]1[NH:8][C:9](=[O:20])[C:10]2[C:15]([CH3:16])=[C:14]([C:17]([O-:19])=[O:18])[S:13][C:11]=2[N:12]=1.[OH-].[Na+].Cl>O.C(O)C>[Cl:2][C:3]1[CH:4]=[C:5]([CH:21]=[CH:22][C:23]=1[Cl:24])[CH2:6][C:7]1[NH:8][C:9](=[O:20])[C:10]2[C:15]([CH3:16])=[C:14]([C:17]([OH:19])=[O:18])[S:13][C:11]=2[N:12]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57821272917089-11-3

Produkt 1

HCID 547559162-(3,4-Dichlorobenzyl)-5-methyl-4-oxo-3,4-dihydrothieno(2,3-d)pyrimidine-6-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

A mixture of 2-(3,4-dichlorobenzyl)-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid mono sodium salt (2.501 g), 1 mol/L aqueous sodium hydroxide solution (9.6 mL) and water (39.4 mL) was dissolved by stirring. The reaction mixture was ice-cooled, ethanol (10 mL) was added, the inside temperature was set to about 2° C., neutralized with 1 mol/L hydrochloric acid (16.0 mL), water (25.0 mL) was added (solvent amount was set to 100 mL), and the mixture was stirred under ice-cooling to confirm that the inside temperature was about 1° C. The suspension was poured into a G2 glass filter (diameter 3 cm), and the pressure reduction was started at 50 hpa. The time necessary to the increase of pressure by the completion of filtration was 42 minutes 52 seconds. The height of the solid at that time was 4.3 cm (bulk 30.4 cm3). Washing with water was not possible due to clogging.

Aufarbeitung

  1. dissolutionwas dissolved
  2. temperaturecooled
  3. customwas set to about 2° C.
  4. additionwas added (solvent amount was set to 100 mL)
  5. stirringthe mixture was stirred under ice-
  6. temperaturecooling
  7. customwas about 1° C
  8. additionThe suspension was poured into a G2 glass
  9. filtrationfilter (diameter 3 cm)
  10. temperatureThe time necessary to the increase of pressure by the completion of filtration
  11. washWashing with water

Quellen und Nachweise

ORD-Eintrag
ord-238af3fd38624b54b6f41cc8720f5156
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08748437B2

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