Dichloromethane → HCID 66671763, Verbindung

Reaktionsgleichung

C(OC([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]#[N:22])=[C:17]([C:23]([F:26])([F:25])[F:24])[CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O.[Cl:34]CCl>>[ClH:34].[NH:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]#[N:22])=[C:17]([C:23]([F:24])([F:25])[F:26])[CH:16]=2)[CH2:10][CH2:9]1

Komponenten

Edukt 3

HCID 6344Dichloromethane

HCID 6422Trifluoroacetic acid

HCID 58576648Tert-butyl 4-[[4-cyano-3-(trifluoromethyl)phenyl]amino]piperidine-1-carboxylate

Produkt 1

HCID 66671763HCID 66671763, Verbindung

Versuchsvorschrift

To a solution of 4-(4-cyano-3-trifluoromethyl-phenylamino)-piperidine-1-carboxylic acid tert-butyl ester (250 mg; 0.68 mmol, prepared in accordance with Example 154) in dichloromethane (5 mL) is added trifluoroacetic acid (1.5 mL) and the reaction mixture is stirred at room temperature for 30 minutes. All volatiles are then removed under high vacuum and the residue is taken up with diethyl ether and concentrated again. The residue is dissolved in a minimum amount of dioxane and a 4 molar solution of hydrochloric acid in dioxane is added. The precipitate formed is collected, washed with diethyl ether and dried under high vacuum to afford the desired compound (225 mg; 0.74 mmol).