Hydrochloric Acid → HCID 58447740, Verbindung

HRID 592242Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 592242
[F:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][C:15]([O:17]CC)=[O:16])=[CH:10][N:9]=2)[CH:5]=[CH:4][N:3]=1.[OH-].[Na+].Cl>C1COCC1.O>[F:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][C:15]([OH:17])=[O:16])=[CH:10][N:9]=2)[CH:5]=[CH:4][N:3]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 58447698Ethyl 2-(2'-fluoro-2,4'-bipyridin-5-yl)acetate

Produkt 1

HCID 58447740HCID 58447740, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

A mixture of ethyl 2-(2′-fluoro-2,4′-bipyridin-5-yl)acetate 208-2 (93 mg, 0.36 mmol) and NaOH (57 mg, 1.43 mmol) in THF (0.5 mL) and water (0.5 mL) was stirred at 65° C. for 3 hours. After cooled down to room temperature, the mixture was treated with 3N HCl aqueous solution to adjust the pH around 3, and then stirred for 15 minutes. The resulting solution was evaporated to dryness and the remaining solid was extracted with 20% methanol in ethyl acetate. The organic portion was concentrated to give 2-(2′-fluoro-2,4′-bipyridin-5-yl)acetic acid 208-3 as pale white solid. MS m/z 233.1 (M+1).

Aufarbeitung

  1. temperatureAfter cooled down to room temperature
  2. stirringstirred for 15 minutes
  3. customThe resulting solution was evaporated to dryness
  4. extractionthe remaining solid was extracted with 20% methanol in ethyl acetate
  5. concentrationThe organic portion was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-bd3991ba35504513a06dda5cfe4af934
Quelldatensatz
uspto-grants-2016_01
Patentnummer
US09238646B2

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