関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Chloro-N,N-dimethyl-1-propanamine | HCID 66960 | — |
| 反応物 | 3-Acetyl-2-(2-hydroxyphenyl)benzothiazoline | HCID 13335960 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Acetyl-2-[2-(3-dimethylaminopropoxy)phenyl]benzothiazoline | HCID 13335759 | 56% |
反応手順
To the suspension of 0.26 g of the sodium hydride in anhydrous DMF, the solution of 1.36 g of 3-acetyl-2-(2-hydroxyphenyl)benzothiazoline in 5 ml of anhydrous DMF is added dropwise under nitrogen atmosphere at room temperature. After the addition, the reaction mixture is stirred for 20 minutes at room temperature. To the reaction mixture, the solution of 0.61 g of 3-dimethylaminopropyl chloride in 10 ml of anhydrous DMF is added. The reaction mixture is stirred for 2 hours at 80° C., and washed with n-hexane after cooling and poured into ice-water. The separated oil is extracted with ethyl acetate. The organic layer is washed with N--NaOH solution, water and saturated sodium chloride solution in the order named and dried over anhydrous magnesium sulfate. Ethy acetate is removed off in vacuo to give 1.0 g (56%) of the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04558125 |
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| 出典データセット | uspto-grants-1985_12 |
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| ORD ID | ord-2bc37b56090748659ea5ce9af168942d |
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| 出典メモ | uspto-grants-1985_12 |
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