Reaktionsgleichung
[H-].[Na+].[CH2:3]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][OH:14])[CH2:4][CH2:5][CH2:6][CH3:7].Br[CH2:16][CH2:17][CH2:18][CH2:19][C:20]#[N:21].Cl>>[C:20](#[N:21])[CH2:19][CH2:18][CH2:17][CH2:16][O:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][O:8][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]Komponenten
5
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
Sodium hydride (60%, 0.75 g) was added to a solution of 3 g of 5-pentyloxy-1-pentanol prepared in the above-described step (1) in 50 ml of N,N-dimetnylformamide. Then 2 ml of 5-bromopentanenitrile was added thereto and the mixture was stirred at 60° C. for 2 h. 3% hydrochloric acid was added to the reaction solution. After extraction with ether, the organic layer was dried and concentrated and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=9/1) to obtain 1 g of the intended product.
Aufarbeitung
- customprepared in the above-described step (1) in 50 ml of N,N-dimetnylformamide
- extractionAfter extraction with ether
- customthe organic layer was dried
- concentrationconcentrated
- customthe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=9/1)
Quellen und Nachweise
- ORD-Eintrag
- ord-d65c5c74758d4904b290441262e7ab08
- Quelldatensatz
- uspto-grants-1991_08
- Patentnummer
- US05037827
Verknüpfte Notizen
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