関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Methoxybenzenesulfonyl chloride | HCID 7401 | — |
| 反応物 | 4-(2-Naphthyl)-thiazol-2-ylamine hydrobromide | HCID 2803037 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 4-methoxy-N-(4-naphthalen-2-yl-thiazol-2-yl)-benzenesulfonamide | HCID 10340709 | 29.4% |
反応手順
A mixture of 0.5 g of 4-(2-naphthyl)-thiazol-2-ylamine hydrobromide with 0.34 g of 4-methoxy-benzenesulfonyl chloride was stirred for 3 hours with 2 ml of pyridine. The resulting, red colored suspension was poured into 30 ml of 1N hydrochloric acid and extracted with ethyl acetate. The organic phases were combined, dried with magnesium sulphate and freed from solvent. The residue was dissolved in a mixture of 25 ml of ethanol and 20 ml of 2N sodium hydroxide solution. After the addition of 0.5 g of active charcoal the mixture was stirred at room temperature for 30 minutes and subsequently the active charcoal was filtered off. The product separated upon neutralization with concentrated hydrochloric acid. Recrystallization from 10 ml of ethyl acetate and 15 ml of n-hexane yielded 0.19 g of 4-methoxy-N-(4-naphthalen-2-yl-thiazol-2-yl)-benzenesulfonamide as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05958910 |
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| 出典データセット | uspto-grants-1999_09 |
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| ORD ID | ord-5fa11970a696472ab5607fde3a83f943 |
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| 出典メモ | uspto-grants-1999_09 |
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