Isopropyl iodide → 1,1-Dimethylethyl 4-{[1-(1-methylethyl)-4-piperidinyl]methyl}-1-piperidinecarboxylate

HRID 1869621Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1869621
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][CH:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)[CH2:3][CH2:2]1.[CH:21](I)([CH3:23])[CH3:22].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH3:22][CH:21]([N:1]1[CH2:2][CH2:3][CH:4]([CH2:7][CH:8]2[CH2:9][CH2:10][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:12][CH2:13]2)[CH2:5][CH2:6]1)[CH3:23]

Komponenten

5

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

1,1-Dimethylethyl 4-(4-piperidinylmethyl)-1-piperidinecarboxylate (may be prepared as described in Description 2) (3 g), isopropyl iodide (3.2 ml) and K2CO3 (2.94 g) were combined in acetonitrile (70 ml) and the reaction mixture heated at 50° C. overnight. The reaction was allowed to cool to room temperature, filtered and evaporated. The residue was dissolved in diethylether (50 ml) and washed successively with water (50 ml), saturated sodium thiosulphate solution (50 ml), saturated brine (50 ml) and dried (Na2SO4). The solvent was evaporated to give the title compound (D3) as a pale yellow oil (3.1 g).

Aufarbeitung

  1. temperatureto cool to room temperature
  2. filtrationfiltered
  3. customevaporated
  4. dissolutionThe residue was dissolved in diethylether (50 ml)
  5. washwashed successively with water (50 ml), saturated sodium thiosulphate solution (50 ml), saturated brine (50 ml)
  6. dry with materialdried (Na2SO4)
  7. customThe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-64d3a6b4d34046f9998aafb24779ff0f
Quelldatensatz
uspto-grants-2009_12
Patentnummer
US07638631B2

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