Lithium Hydroxide → 6-Methyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carboxylic acid

HRID 1260304Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1260304
C([O:3][C:4]([C:6]1[C:11]([NH:12][C:13]2[CH:14]=[N:15][CH:16]=[N:17][CH:18]=2)=[N:10][CH:9]=[C:8]([CH3:19])[N:7]=1)=[O:5])C.[OH-].[Li+]>C1COCC1.C(O)C>[CH3:19][C:8]1[N:7]=[C:6]([C:4]([OH:5])=[O:3])[C:11]([NH:12][C:13]2[CH:18]=[N:17][CH:16]=[N:15][CH:14]=2)=[N:10][CH:9]=1

Komponenten

4

Edukt 2

HCID 3939Lithium HydroxideHCID 673001846-Methyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carboxylic acid ethyl ester

Produkt 1

HCID 583680556-Methyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carboxylic acidAusbeute 69,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21873804Tetrahydrofuran ethanolLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

6-Methyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carboxylic acid ethyl ester (300 mg, 1.15 mmol) was dissolved in a THF/ethanol (5 ml/1 ml) mixture, cooled to 0° C. and treated with lithium hydroxide (4.7 ml, 1N aqueous solution). The reaction mixture was allowed to warms to ambient temperature and stirred at that temperature for 1 hour. The pH value was subsequently adjusted to acidic and the resulting suspension was filtrated. The precipitate was washed with water and ethyl acetate and dried to yield the product as light yellow solid (185 mg, 69%).

Aufarbeitung

  1. customwas allowed to warms to ambient temperature
  2. filtrationwas filtrated
  3. washThe precipitate was washed with water and ethyl acetate
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a5644691a59f43d2859a0ae977941b2b
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08470820B2

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