Trifluoroacetic acid → 5-Chloro-2-(piperazin-1-yl)benzonitrile

HRID 457163

Reaktionsgleichung

Reaktionsgleichung von HRID 457163
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=2[C:21]#[N:22])[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[Cl:20][C:17]1[CH:18]=[CH:19][C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)=[C:15]([CH:16]=1)[C:21]#[N:22]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 667578634-(4-Chloro-2-cyano-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 193671275-Chloro-2-(piperazin-1-yl)benzonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 4-(4-chloro-2-cyano-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (0.32 g, 1 mmol) in dichloromethane cooled at 0° C. was treated with trifluoroacetic acid (20%) and warmed to room temperature and stirred for 2 h. The reaction mixture was concentrated in vacuo, diluted with ethyl acetate and free based with 10% aqueous sodium bicarbonate. The organic layers were separated and dried over sodium sulfate and concentrated in vacuo. The product used without further purification.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. customThe organic layers were separated
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe product used without further purification

Quellen und Nachweise

ORD-Eintrag
ord-363384bf4dbc4f68ad8ab2d2e61bd5c8
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07186729B2

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