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HRID 36906作成日:2026年10月23日
alpha-chloro-N,N-dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride → N,N-Dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]-benzothiazole-3-acetamide
https://huagongshe.com/ja/reaction/36906
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | alpha-chloro-N,N-dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride | HCID 19936710 | — |
| 反応物 | Sodium Formaldehyde Sulfoxylate | HCID 23689980 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N,N-Dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]-benzothiazole-3-acetamide | HCID 9884996 | 71.7% |
反応手順
40 g (0.0938 mole) of α-chloro-N,N-dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride in solution in 1200 ml of dichloromethane are treated with 43.6 (0.283 mole) of Rongalite®, while stirring the mixture at room temperature for 6 h. The suspension is filtered, it is rinsed with dichloromethane and the organic phase is washed (pH=1) with 500 ml of 0.5N sodium hydroxide up to a pH>10, then to neutral pH with a saturated sodium chloride solution. The organic phase is dried over sodium sulphate and the solvent is evaporated under reduced pressure. A beige-coloured solid is obtained which is purified by chromatography on a silica gel column, eluting with a 95/5 mixture of dichloromethane/methanol. 23.9 g of a white solid are obtained. Melting point: 216°-218° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05418248 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-edf4702c5b204ea8b368e24852d3b023 |
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| 出典メモ | uspto-grants-1995_05 |
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