Lithium Hydroxide → 4-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid lithium salt

HRID 511066Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 511066
C([O:3][C:4](=[O:24])[CH2:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)C.[OH-].[Li+:26]>O1CCCC1.O.C(#N)C>[Li+:26].[F:23][C:20]([F:21])([F:22])[C:17]1[CH:18]=[CH:19][C:14]([N:11]2[CH2:12][CH2:13][N:8]([CH2:7][CH2:6][CH2:5][C:4]([O-:24])=[O:3])[CH2:9][CH2:10]2)=[CH:15][CH:16]=1

Komponenten

6

Edukt 2

HCID 3939Lithium HydroxideHCID 585765934-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester

Produkt 1

HCID 585760704-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid lithium salt

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

4-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester (660 mg; 1.92 mmol, prepared in accordance with Example 2) and lithium hydroxide are dissolved in a mixture of tetrahydrofuran (2.8 mL) and water (1.2 mL). The resulting mixture is irradiated in a mono-mode microwave oven for 30 minutes at 70° C. The mixture is then diluted with acetonitrile (20 mL) and the precipitate formed is filtered and rinsed with acetonitrile (10 mL). The solid obtained is then dried under high vacuum to deliver the desired product (584 mg; 1.81 mmol).

Aufarbeitung

  1. customThe resulting mixture is irradiated in a mono-mode microwave oven for 30 minutes at 70° C
  2. customthe precipitate formed
  3. filtrationis filtered
  4. washrinsed with acetonitrile (10 mL)
  5. customThe solid obtained
  6. customis then dried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-ce965d0904984e019d4eeca57770a8e7
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09096524B2

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