関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3,5-Tris(bromomethyl)benzene | HCID 530258 | — |
| 反応物 | 2-((Triphenylmethyl)amino)ethanol | HCID 3125608 | — |
| 反応物 | 4-(5-Chlorosulfonyl-2,4-dimethoxyphenyl)-2,6-pyridine dicarboxylic acid dimethyl ester | HCID 15001916 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Chloroform methanol | HCID 21584188 | — |
| 生成物 | 4-(2,4-Dimethoxyphenyl)pyridine-2,6-dicarboxylic Acid | HCID 15001914 | — |
反応手順
To a suspension of 0.5 g (0.0008 mole) of the amine-hydrochloride 8 in 20 ml of CH2Cl2 was added all at once 1.4 ml (0.01 mole) of Et3N. The mixture was then cooled to 5°-10° C. and 1.4 g (0.0032 mole) of the sulfonyl chloride 39 in 20 ml of CH2Cl2 was slowly added in a dropwise fashion. The reaction was then allowed to stir at room temperature for 30 minutes after which a TLC was taken. Little of the sulfonyl chloride 9 had reacted by TLC so an additional 100 mg of the amine 8 was added and stirring continued overnight. The mixture was then poured into water and extracted with CH2Cl2. The extract was washed with water, dried (Na2SO4) and the solvent removed yielding crude 43. After column chromatography with SiO2 /5%MeOH/CHCl3, 1.55 g (93%) of the desired tetraamide 43 was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05245038 |
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| 出典データセット | uspto-grants-1993_09 |
|---|
| ORD ID | ord-1c4af60950e34e5ba3caea2d9484da0b |
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| 出典メモ | uspto-grants-1993_09 |
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