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Thiophosgene → 2-Tert-butyl-6-isothiocyanato-5-(4-methyl-piperazin-1-yl)benzothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophosgene | HCID 10040 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-Amino-2-tert-butyl-5-(4-methylpiperazin-1-yl)benzothiazole | HCID 19794176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Tert-butyl-6-isothiocyanato-5-(4-methyl-piperazin-1-yl)benzothiazole | HCID 19794187 | — |
反応手順
To a stirred mixture of 75 g of 6-Amino-2-tert-butyl-5-(4-methylpiperazin-1-yl)benzothiazole and 29 g of sodium bicarbonate in 1100 ml of chloroform at 0° is added 41 g of thiophosgene and the mixture stirred at 10° for 4 hours. After filtering off the solid, the solution is evaporated to get a yellow solid which is dissolved in water and the pH of the solution is brought to 7 by the addition of dilute sodium hydroxide. The solid separated is extracted with hexane and filtered through 150 g of neutral alumina to give 2-tert-butyl-6-isothiocyanato-5-(4-methyl-piperazin-1-yl)benzothiazole, melting at 124°-126°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246927 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-a9b6c5936caf4afa829011ebb019f26e |
| 出典メモ | uspto-grants-1993_09 |