Hydrochloric Acid → 1-(2-Fluoro-4-(trifluoromethyl)phenyl)piperazine

HRID 32655Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 32655
C(OC([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][C:15]=2[F:24])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>O1CCOCC1>[F:24][C:15]1[CH:16]=[C:17]([C:20]([F:21])([F:22])[F:23])[CH:18]=[CH:19][C:14]=1[N:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 534855174-(2-Fluoro-4-trifluoromethylphenyl)piperazine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 468374951-(2-Fluoro-4-(trifluoromethyl)phenyl)piperazineAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

A mixture of 3.11 g (9 mmol) 4-(2-Fluoro-4-trifluoromethyl-phenyl)-piperazine-1-carboxylic acid tert-butyl ester in 20 ml dioxane was treated with 8.93 ml 4N HCl in dioxane for 2 h at 80° C. The mixture was concentrated and treated with 20 ml water, 20 ml 2M Na2CO3 and extracted with 50 ml EtOAc. The organic phase was washed with 30 ml saturated NaCl. All aqueous phases were combined and extracted with 50 ml EtOAc. The combined organic phases were dried with MgSO4 and evaporated to yield 2.1 g (95%) of the title compound as brownish crystals.

Aufarbeitung

  1. concentrationThe mixture was concentrated
  2. additiontreated with 20 ml water, 20 ml 2M Na2CO3
  3. extractionextracted with 50 ml EtOAc
  4. washThe organic phase was washed with 30 ml saturated NaCl
  5. extractionextracted with 50 ml EtOAc
  6. dry with materialThe combined organic phases were dried with MgSO4
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-ec79806d7bf3432c93dc9e1236a2f601
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07427612B2

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