Ammonia → HCID 18668788, Verbindung
Reaktionsgleichung
[CH2:1]1[CH2:13][O:12][C:3]2([CH2:8][CH2:7][N:6]([CH2:9][C:10]#[N:11])[CH2:5][CH2:4]2)[O:2]1.N>[Ni]>[NH2:11][CH2:10][CH2:9][N:6]1[CH2:5][CH2:4][C:3]2([O:12][CH2:13][CH2:1][O:2]2)[CH2:8][CH2:7]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A suspension of 12.7 g of 4,4-ethylenedioxy-1-piperidineacetonitrile, 1.3 ml of Raney nickel and 113 ml of 2% methanolic solution of ammonia was catalytically hydrogenated at room temperature under 50 atm for 20 hours. After the reaction, the catalyst was filtered off, and the filtrate was concentrated. The resulting pale green liquid was purified by alumina column chromatography [eluting solvent: ethyl acetate→ethyl acetate—methanol (10:1)] to give 10.1 g of a colorless liquid.
Aufarbeitung
- customAfter the reaction
- filtrationthe catalyst was filtered off
- concentrationthe filtrate was concentrated
- customThe resulting pale green liquid was purified by alumina column chromatography [eluting solvent: ethyl acetate→ethyl acetate—methanol (10:1)]
Quellen und Nachweise
- ORD-Eintrag
- ord-80eab6727b4b4bb39dad5bc0f5280330
- Quelldatensatz
- uspto-grants-2003_02
- Patentnummer
- US06518265B1
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