関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 5-Methoxy-2-[4-(2-chloroethoxy)anilino]benzothiazole | HCID 21538599 | — |
| 溶媒 | 2-Methoxyethanol | HCID 8019 | — |
| 生成物 | Benzothiazole, 5-methoxy-2-(beta-(1-pyrrolidinyl)-p-phenetidino)- | HCID 38054 | — |
反応手順
A mixture of 5-methoxy-2-[4-(2-chloroethoxy)anilino]benzothiazole (200 g.), pyrrolidine (144 ml.) and 2-methoxyethanol (1 liter) is boiled under reflux for 16 hours. The mixture is evaporated from the steam bath at reduced pressure and the residue dissolved in approximately 2N hydrochloric acid. The solution is washed with ethyl acetate, basified with 40% sodium hydroxide solution and extracted with chloroform. The chloroform is washed with water, dried over magnesium sulphate and passed through a column of alumina. The column is washed with chloroform and the combined chloroform solutions evaporated. The residue is recrystallised from 2-methoxyethanol to give 5-methoxy-2-[4-(2-pyrrolidin-1-ylethoxy)anilino]benzothiazole, m.p. 167° - 168°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03957999 |
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| 出典データセット | uspto-grants-1976_05 |
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| ORD ID | ord-7b807eee5d1a450c9885bdbf191aba69 |
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| 出典メモ | uspto-grants-1976_05 |
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