関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | Ethyl 2-aminothiazole-4-carboxylate | HCID 73216 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Ethyl 2-tritylaminothiazole-4-carboxylate | HCID 15053536 | — |
反応手順
A mixture comprising 5 g of triphenylchloromethane and 15 ml of dichloromethane was added dropwise at -30° C. to a mixture comprising 3.1 g of ethyl 2-aminothiazole-4-carboxylate, 25 ml of dimethylformamide and 1.8 g of triethylamine. The reaction mixture was maintained at -30° C. for 10 minutes and was then stirred at room temperature for 2 hours. after which it was poured into ice water and extracted with ethyl acetate. The extract was washed successively with 0.1N hydrochloric acid and aqueous sodium chloride solution, and then dried over anhydrous sodium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by silica gel chromatography, using as eluent a 10:1 by volume mixture of benzene and ethyl acetate. The crystals obtained thereby were washed with n-hexane, to afford the desired compound as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04933355 |
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| 出典データセット | uspto-grants-1990_06 |
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| ORD ID | ord-2b08955f6dea42c8988b651be9efa87f |
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| 出典メモ | uspto-grants-1990_06 |
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