Sodium Hydroxide → 1-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine

HRID 2263263

Reaktionsgleichung

Reaktionsgleichung von HRID 2263263
Cl.[F:2][C:3]1[C:8]([F:9])=[CH:7][CH:6]=[CH:5][C:4]=1[C:10]1[N:11]=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)[S:13][CH:14]=1.[OH-].[Na+]>O>[F:2][C:3]1[C:8]([F:9])=[CH:7][CH:6]=[CH:5][C:4]=1[C:10]1[N:11]=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)[S:13][CH:14]=1

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 687762881-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride

Produkt 1

HCID 687762891-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazineAusbeute 56,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A 4 N solution (50 ml) of hydrogen chloride in ethyl acetate was added to a solution of tert-butyl 4-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine-1-carboxylate (4.20 g, 11.0 mmol) in ethyl acetate (100 ml), and the mixture was stirred at room temperature for 14 hours. Hexane was added to the reaction mixture, and crystals were collected by filtration to give 1-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride. The hydrochloride was dissolved in water, neutralized with a 1 N sodium hydroxide aqueous solution, and extracted with chloroform. The extract was washed with water, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give 1.76 g (56.8%) of the desired product as a solid.

Aufarbeitung

  1. extractionextracted with chloroform
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a0dc484bb6a1418eaf18f6d2c2bc8459
Quelldatensatz
uspto-grants-2010_12
Patentnummer
US07851473B2

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