Lithium Hydroxide → 7-Carboxy-6,7-dihydro-1-methylpyrazolo[3,4-d]thiazolo[3,2-a]pyrimidin-4(1H)-one

HRID 260521Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 260521
C([O:3][C:4]([CH:6]1[S:19][C:9]2=[N:10][C:11]3[N:17]([CH3:18])[N:16]=[CH:15][C:12]=3[C:13](=[O:14])[N:8]2[CH2:7]1)=[O:5])C.[OH-].[Li+]>O1CCOCC1.O>[C:4]([CH:6]1[S:19][C:9]2=[N:10][C:11]3[N:17]([CH3:18])[N:16]=[CH:15][C:12]=3[C:13](=[O:14])[N:8]2[CH2:7]1)([OH:5])=[O:3]

Komponenten

5

Edukt 2

HCID 3939Lithium HydroxideHCID 224016666,7-Dihydro-7-ethoxycarbonyl-1-methylpyrazolo[3,4-d]thiazolo[3,2-a]pyrimidin-4(1H)-one

Produkt 1

HCID 224016787-Carboxy-6,7-dihydro-1-methylpyrazolo[3,4-d]thiazolo[3,2-a]pyrimidin-4(1H)-oneAusbeute 69,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

In a mixture of 50 ml of dioxane and 14 ml of water was dissolved 1.30 g (6.24 mmol) of Compound 42 prepared in Example 33, and 0.52 g (12.5 mmol) of lithium hydroxide was added to the solution, followed by stirring at room temperature for 30 minutes. After evaporation of the solvent, the residue was dissolved in water, and then hydrochloric acid was added. The precipitated crystals were collected by filtration, and washed with water, followed by recrystallization from dimethylformamide/water to give 1.09 g (69%) of Compound 43.

Aufarbeitung

  1. additionwas added to the solution
  2. customAfter evaporation of the solvent
  3. dissolutionthe residue was dissolved in water
  4. additionhydrochloric acid was added
  5. filtrationThe precipitated crystals were collected by filtration
  6. washwashed with water
  7. customfollowed by recrystallization from dimethylformamide/water

Quellen und Nachweise

ORD-Eintrag
ord-1931353db06848b5b673f174666e7ee4
Quelldatensatz
uspto-grants-1996_06
Patentnummer
US05527908

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