Reaktionsgleichung
[CH:1](=[N+:8]([O-:16])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[P:17]([O:44]CCCCCCCCCCCC)([O:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])[O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30].[CH2:57](I)[CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH2:64][CH2:65][CH2:66][CH2:67][CH3:68]>>[CH2:1]([N:8]([CH:9]([P:17](=[O:44])([O:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])[O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[O:16][CH2:68][CH2:67][CH2:66][CH2:65][CH2:64][CH2:63][CH2:62][CH2:61][CH2:60][CH2:59][CH2:58][CH3:57])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
A mixture of 5.0 g (23 mmol) of N-benzylidenebenzylamine N-oxide, 17.6 g (30 mmol) of tri-n-dodecyl phosphite and 29.6 g (100 mmol) of n-dodecyl iodide is heated at 70° C. for 24 hours. The reaction mixture is concentrated in vacuo and the residue is purified by HPLC (4:1 hexane:ethyl acetate eluent) followed by flash chromatography (methylene chloride eluent) to give 5.1 g (28% yield) of the title compound as a white solid melting at 38°-40° C.
Aufarbeitung
- concentrationThe reaction mixture is concentrated in vacuo
- customthe residue is purified by HPLC (4:1 hexane:ethyl acetate eluent)
Quellen und Nachweise
- ORD-Eintrag
- ord-e2ae07b1df9d489c892af2630f965bde
- Quelldatensatz
- uspto-grants-1991_12
- Patentnummer
- US05077329
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