Sodium Hydroxide → 2-(4,6-Dimethyl-5-nitropyrimidine-2-ylamino)acetic acid

HRID 1749266Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1749266
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[N:5]=[C:4]([NH:12][CH2:13][C:14]([O:16]CC)=[O:15])[N:3]=1.[OH-].[Na+]>O1CCOCC1>[CH3:11][C:6]1[C:7]([N+:8]([O-:10])=[O:9])=[C:2]([CH3:1])[N:3]=[C:4]([NH:12][CH2:13][C:14]([OH:16])=[O:15])[N:5]=1

Komponenten

4

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

Compound 10 (80 mg) was suspended in 1,4-dioxane (1.5 mL) and a 2N aqueous sodium hydroxide solution (1.5 mL) was added at room temperature (20 to 30° C.). The mixture was stirred at room temperature (20 to 30° C.) for 8 hours. Subsequently, the mixture was washed with diethyl ether. While the reaction mixture was cooled, a 2N aqueous HCl solution was added portionwise to neutralize the mixture to a pH of 3. The mixture was extracted twice with chloroform and the organic layer was concentrated under reduced pressure to give 52 mg (75% yield) of the desired product as a pale yellow amorphous.

Aufarbeitung

  1. washSubsequently, the mixture was washed with diethyl ether
  2. temperatureWhile the reaction mixture was cooled
  3. additiona 2N aqueous HCl solution was added portionwise
  4. extractionThe mixture was extracted twice with chloroform
  5. concentrationthe organic layer was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-66d5b3d38c6441469237eff69c018d3d
Quelldatensatz
uspto-grants-2015_10
Patentnummer
US09156817B2

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