関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 2-Aminomethyl-1-ethylpyrrolidine | HCID 117295 | — |
| 反応物 | 3,5-Dichloro-2,6-dimethoxybenzoic Acid | HCID 2774750 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Benzamide, 3,5-dichloro-2,6-dimethoxy-N-(1-ethyl-2-pyrrolidinylmethyl)- | HCID 54941 | — |
反応手順
20 ml of thionyl chloride is added to 11.9 g (0.047 mol) of 3,5-dichloro-2,6-dimethoxybenzoic acid. The mixture is heated on a steam bath for 30 minutes. To the solution is added 50 ml of toluene. The solvent and excess thionyl chloride is evaporated at reduced pressure. The residue is dissolved in 50 ml of dry ethyl ether. To the obtained solution is added dropwise while stirring 6.0 g (0.047 mol) of 2-(aminomethyl)-1-ethylpyrrolidine in 50 ml of ethyl ether. After 30 minutes at room temperature 300 ml of water is added while stirring. The water layer is separated and alkalized with sodium hydroxide solution which is added dropwise while stirring and cooling in ice. The precipitate is collected and washed with water. Yield: 9.0 g, m.p. 120°-21° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04232037 |
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| 出典データセット | uspto-grants-1980_11 |
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| ORD ID | ord-b3b738a827e8417e8e72b8888fb1ea24 |
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| 出典メモ | uspto-grants-1980_11 |
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