Lithium Hydroxide → HCID 57471876, Verbindung

HRID 1802001Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1802001
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([N:15]3[CH:19]=[CH:18][CH:17]=[N:16]3)=[C:11]([F:20])[CH:10]=2)[C:5]([C:21]([O:23]CC)=[O:22])=[CH:4][N:3]=1.[Li+].[OH-]>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([N:15]3[CH:19]=[CH:18][CH:17]=[N:16]3)=[C:11]([F:20])[CH:10]=2)[C:5]([C:21]([OH:23])=[O:22])=[CH:4][N:3]=1

Komponenten

4

Edukt 2

HCID 3939Lithium HydroxideHCID 59199531HCID 59199531, Verbindung

Produkt 1

HCID 57471876HCID 57471876, VerbindungAusbeute 90,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of ethyl 2-chloro-4-(3-fluoro-4-(1H-pyrazol-1-yl)phenylamino)pyrimidine-5-carboxylate (275 mg, 0.761 mmol) in THF (4 mL), aq. 1N LiOH (1.25 mL, 1.25 mmol) was added. The mixture was stirred at room temperature overnight. Upon acidification of the mixture with 1N HCl, white solids precipitated out, which were collected, and dried on vacuum to give 2-chloro-4-(3-fluoro-4-(1H-pyrazol-1-yl)phenylamino)pyrimidine-5-carboxylic acid (230 mg). MS 334.3 and 336.3 (M+H, Cl pattern)

Aufarbeitung

  1. customUpon acidification of the mixture with 1N HCl, white solids precipitated out
  2. customwhich were collected
  3. customdried on vacuum

Quellen und Nachweise

ORD-Eintrag
ord-0a7aec6e4ce349499106bfb8329a1e1c
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08349860B2

Notizen zur Reaktion

Wird geladen…