関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 4-Chloro-3-sulfamoylbenzoic acid | HCID 14568 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-(2-Methoxyphenyl)piperazin-1-amine | HCID 13730200 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Chloro-N-[4-(2-methoxyphenyl)-1-piperazinyl]-3-sulfamoylbenzamide | HCID 13730201 | — |
反応手順
To a solution of 1.8 g of N,N'-dicyclohexylcarbodiimide in 5 ml tetrahydrofuran was added a solution of 2.1 g of 4-chloro-3-sulfamoylbenzoic acid in 20 ml of tetrahydrofuran under stirring at room temperature. After the addition was completed, the mixture was stirred at room temperature for 20 minutes, then 0.83 g of 1-amino-4-(2-methoxyphenyl)piperazine was added, and the reaction mixture was stirred for 5 hours. Then 5 ml of 10% hydrochloric acid was added and stirred at room temperature for 10 minutes. 250 ml of 2% sodium hydroxide solution was added and insoluble materials were filtered off. The filtrate was alkalized with 2% sodium hydroxide solution to give white precipitate. The resulting precipitate was filtered, washed with water and recrystallized from ethanol to afford a title compound in a yield of 0.84 g (49%) as colorless crystals, mp 232°-235° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04650871 |
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| 出典データセット | uspto-grants-1987_03 |
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| ORD ID | ord-411647cc998e4d4ca62539f7a7fc43cd |
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| 出典メモ | uspto-grants-1987_03 |
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