Reaktionsgleichung
[CH3:1][N:2]([CH3:18])[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[O:17])[C:8]1[CH:13]=[CH:12][C:11]([N:14]([CH3:16])[CH3:15])=[CH:10][CH:9]=1.[CH2:19]([O:37][S:38]([C:41]1[CH:46]=[CH:45][C:44]([CH3:47])=[CH:43][CH:42]=1)(=[O:40])=[O:39])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]C.[CH2:48](OC(=O)C)C>>[C:44]1([CH3:47])[CH:43]=[CH:42][C:41]([S:38]([O-:40])(=[O:37])=[O:39])=[CH:46][CH:45]=1.[CH2:18]([N+:2]([CH2:3][CH2:4][CH2:5][NH:6][C:7](=[O:17])[C:8]1[CH:9]=[CH:10][C:11]([N:14]([CH3:16])[CH3:15])=[CH:12][CH:13]=1)([CH3:48])[CH3:1])[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH3:19]Komponenten
Versuchsvorschrift
N-(3-dimethylaminopropyl)-p-dimethylaminobenzamide (77 g, 0.31 mole) from Example 1 and 131.5 g of stearyl-p-toluenesulfonate (0.31 mole) was heated to 110° C. under a blanket of nitrogen with continuous stirring for 2 hours. The resulting melt was dissolved in 800 ml of hot ethylacetate and then crystallized by cooling to ambient temperature. The crystals were recovered by filtration, dried in air and then under vacuum at 50°-60° C. The resulting whitish crystals of stearyl-[3-(p-dimethyl-aminobenzamido)propyl]dimethyl ammonium p-toluenesulfonate were found to have a melting point of 122°-125° C. and the yield 191.8 g, was 92% of theoretical. The structure and purity of the product were confirmed by elemental analysis, NMR, FTIR and UV spectra.
Aufarbeitung
- customcrystallized
- filtrationThe crystals were recovered by filtration
- customdried in air
- customat 50°-60° C
Quellen und Nachweise
- ORD-Eintrag
- ord-a41d129298094c218abea644cb34c047
- Quelldatensatz
- uspto-grants-1995_09
- Patentnummer
- US05451394
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