関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Octadecyl p-Toluenesulfonate | HCID 229551 | — |
| 反応物 | 4-(dimethylamino)-N-[3-(dimethylamino)propyl]benzamide | HCID 3978888 | — |
| 生成物 | Stearyl-[3-(p-dimethylaminobenzamido) propyl]-Dimethylammonium p-toluenesulfonate | HCID 19382935 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05451394 |
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| 出典データセット | uspto-grants-1995_09 |
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| ORD ID | ord-a41d129298094c218abea644cb34c047 |
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| 出典メモ | uspto-grants-1995_09 |
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