Hydrochloric Acid → 4-(Trifluoromethyl)cyclohexan-1-amine hydrochloride

HRID 2060870Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2060870
C([NH:8][CH:9]1[CH2:14][CH2:13][CH:12]([C:15]([F:18])([F:17])[F:16])[CH2:11][CH2:10]1)C1C=CC=CC=1.[ClH:19]>CO.O1CCOCC1.[Pd]>[ClH:19].[F:16][C:15]([F:17])([F:18])[CH:12]1[CH2:11][CH2:10][CH:9]([NH2:8])[CH2:14][CH2:13]1

Komponenten

6

Edukt 2

HCID 313Hydrochloric AcidHCID 43434579Benzyl(4-trifluoromethylcyclohexyl)amine

Produkt 1

HCID 187699224-(Trifluoromethyl)cyclohexan-1-amine hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of benzyl(4-trifluoromethylcyclohexyl)amine (Preparation 4) (1.48 g, 5.73 mmol) in MeOH (150 mL) was passed through an H-Cube at 100° C. fitted with a 10% Pd/C CatCart and on full H2 mode. The volume was reduced to 50 mL and 4M HCl in dioxane (1.43 mL) was added. The precipitate was filtered, the filtrate collected and the solvent removed in vacuo. The resulting residue was triturated with acetone to give the title compound: δH (CD3OD) 1.41-1.53 (4H, m), 2.03-2.25 (5H, m), 3.07-3.15 (1H, m).

Aufarbeitung

  1. customwas passed through an H-Cube at 100° C.
  2. additionwas added
  3. filtrationThe precipitate was filtered
  4. customthe filtrate collected
  5. customthe solvent removed in vacuo
  6. customThe resulting residue was triturated with acetone

Quellen und Nachweise

ORD-Eintrag
ord-2d9a4257b37e4839b42c5275f1a5e409
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08278442B2

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