Reaktionsgleichung
O[N:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.Cl.[C:9]1(=O)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.[C-:16]#[N:17].[K+].[OH2:19]>>[C:16]([C:9]1([N:2]2[CH2:7][CH2:6][CH:5]([OH:19])[CH2:4][CH2:3]2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)#[N:17]Komponenten
6
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
4 hydroxypiperidine (Aldrich Chemical Co., Inc., supra) (5q) was dissolved in distilled water (14 mL), cooled to 0° C. and the pH was adjusted to between 4 and 5 by addition of concentrated hydrochloric acid and 4 hydroxypiperidine. After warming to room temperature, 5.2 mL cyclohexanone and 3.3 g potassium cyanide in water (9 mL) were added sequentially. After 18 hours of stirring at room temperature, the solid was filtered. The solid was dissolved in 100 mL methylene chloride, dried over Na2SO4, filtered and the solvent was removed in vacuo to yield pure 1 (1 cyanocyclohexyl) 4 hydroxypiperidine.
Aufarbeitung
- temperatureAfter warming to room temperature
- filtrationthe solid was filtered
- dissolutionThe solid was dissolved in 100 mL methylene chloride
- dry with materialdried over Na2SO4
- filtrationfiltered
- customthe solvent was removed in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-a4eb416b22e64863aba5506a62cab93e
- Quelldatensatz
- uspto-grants-1992_10
- Patentnummer
- US05155212
Verknüpfte Notizen
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