Hydrochloric Acid → 3-(2-Piperazin-1-yl-1,3-thiazol-4-yl)benzonitrile

HRID 2263280Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2263280
Cl.[C:2]([C:4]1[CH:5]=[C:6]([C:10]2[N:11]=[C:12]([N:15]3[CH2:20][CH2:19][N:18](C(OC(C)(C)C)=O)[CH2:17][CH2:16]3)[S:13][CH:14]=2)[CH:7]=[CH:8][CH:9]=1)#[N:3]>C(OCC)(=O)C>[N:15]1([C:12]2[S:13][CH:14]=[C:10]([C:6]3[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=3)[C:2]#[N:3])[N:11]=2)[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 68779422Tert-butyl 4-[4-(3-cyanophenyl)-1,3-thiazol-2-yl]piperazine-1-carboxylate

Produkt 1

HCID 639931083-(2-Piperazin-1-yl-1,3-thiazol-4-yl)benzonitrileAusbeute 65,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel2×

Versuchsvorschrift

A 4 N solution (25 ml) of hydrogen chloride in ethyl acetate was added to a solution of tert-butyl 4-[4-(3-cyanophenyl)-1,3-thiazol-2-yl]piperazine-1-carboxylate (920 mg, 2.48 mmol) in ethyl acetate (50 ml), the mixture was stirred at room temperature for 6 hours, and the solvent was distilled off under reduced pressure. The residue 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 438 mg (65.2%) of the desired product as a solid.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-fe456f4770af41c49824d40968ff85e4
Quelldatensatz
uspto-grants-2010_12
Patentnummer
US07851473B2

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