4-(3,4-Dichlorophenoxy)piperidine → Ammonia

HRID 1292754Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1292754
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.CS(O[CH2:21][CH:22]1[O:27][CH2:26][CH2:25][N:24]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:23]1)(=O)=O>C(#N)C>[NH3:9].[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:21][CH:22]2[O:27][CH2:26][CH2:25][N:24]([C:28]([O:30][C:31]([CH3:32])([CH3:34])[CH3:33])=[O:29])[CH2:23]2)[CH2:8][CH2:7]1

Komponenten

5

Edukt 2

HCID 37320424-(3,4-Dichlorophenoxy)piperidineHCID 57791474Tert-butyl 2-(((methylsulfonyl)oxy)methyl)morpholine-4-carboxylate

Produkt 2

HCID 222AmmoniaHCID 17974804tert-Butyl 2-{[4-(3,4-dichlorophenoxy)piperidin-1-yl}methyl]morpholine-4-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of the product from Example 1, Step (b) dissolved in acetonitrile (12 ml) was added the product of Example 2, Step (a). The mixture was refluxed for 12 hrs and the solvents were evaporated. Purification by flash chromatography (silica) eluting with dichloromethane: methanol: NH3 (aq) (2:98:0.1) gave the sub-title compound as an oil (1.9 g).

Aufarbeitung

  1. temperatureThe mixture was refluxed for 12 hrs
  2. customthe solvents were evaporated
  3. customPurification by flash chromatography (silica)
  4. washeluting with dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-035fcec48b814741adcef02eb7c64b74
Quelldatensatz
uspto-grants-2007_07
Patentnummer
US07238691B2

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