Hydrochloric Acid → HCID 69656069, Verbindung

HRID 11684Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 11684
C([O:3][C:4](=[O:34])[CH2:5][CH2:6][C:7]1[C:8]([O:14][CH2:15][C:16]([N:18]2[CH2:23][C@H:22]([CH3:24])[N:21]([CH2:25][C:26]3[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=3)[CH2:20][C@H:19]2[CH3:33])=[O:17])=[N:9][CH:10]=[C:11]([Cl:13])[CH:12]=1)C.O.[OH-].[Li+].Cl.P([O-])([O-])([O-])=O>O1CCCC1.CO.O>[Cl:13][C:11]1[CH:12]=[C:7]([CH2:6][CH2:5][C:4]([OH:34])=[O:3])[C:8]([O:14][CH2:15][C:16]([N:18]2[CH2:23][C@H:22]([CH3:24])[N:21]([CH2:25][C:26]3[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=3)[CH2:20][C@H:19]2[CH3:33])=[O:17])=[N:9][CH:10]=1

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 1061PhosphateHCID 168937Lithium hydroxide, monohydrateHCID 69655855HCID 69655855, Verbindung

Produkt 1

HCID 69656069HCID 69656069, VerbindungAusbeute 25,4 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 3-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-pyridin-3-yl)-propionic acid ethyl ester (0.081 g, 0.17 mmol) in tetrahydrofuran (2 mL), methanol (2 mL) and water (1 mL) was added lithium hydroxide monohydrate (0.013 g, 0.32 mmol). The reaction mixture was stirred at ambient temperature for 3 hours, neutralized with 0.2M hydrochloric acid and phosphate buffer (pH=7), and extracted with ethy acetate. The combined organics were dried over magnesium sulfate, filtered and concentrated in vacuo. Purification with via HPLC gave the title compound (0.020 g, LRMS: 464.4).

Aufarbeitung

  1. extractionextracted with ethy acetate
  2. dry with materialThe combined organics were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customPurification with via HPLC

Quellen und Nachweise

ORD-Eintrag
ord-68e99a9f7abe4ad6afcd22c1448cb0c6
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07098212B2

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