HCID 23081330, Verbindung → HCID 17825545, Verbindung

HRID 856069Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 856069
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:23]=[CH:22][C:6]([CH2:7][O:8][CH:9]2[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1>C(Cl)Cl.FC(F)(F)C(O)=O>[F:25][C:2]([F:1])([F:24])[C:3]1[CH:23]=[CH:22][C:6]([CH2:7][O:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:5][CH:4]=1

Komponenten

4

Versuchsvorschrift

Tert-butyl 4-(4-trifluoromethylbenzyloxy)-piperidine-1-carboxylate (2.56 g, 7.12 mmol) prepared in Reference Example 122 was dissolved in methylene chloride (20 ml), to which trifluoroacetic acid (10 ml) was added dropwise, and the mixture was stirred at room temperature for 5 hours. The reaction mixture was concentrated under reduced pressure, and the residue was then dissolved in methylene chloride. This solution was neutralized with sodium hydroxide aqueous solution and the mixture was extracted with methylene chloride. The extract was washed with brine, dried over magnesium sulfate, and then filtered. The filtrate was concentrated under reduced pressure to afford 4-(4-trifluoromethylbenzyloxy)piperidine (1.85 g, yield 99%) as a white powder.

Aufarbeitung

  1. additionwas added dropwise
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionthe residue was then dissolved in methylene chloride
  4. extractionthe mixture was extracted with methylene chloride
  5. washThe extract was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7c94c5d3849b495e9ab4c773d5cf0c10
Quelldatensatz
uspto-grants-2007_08
Patentnummer
US07262212B2

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