関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 3-tert-Butoxycarbonylamino-5-(1-hydroxy-cyclohexyl)-thiophene-2-carboxylic acid methyl ester | HCID 57795388 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Cyclohex-1-enyl-3-aminothiophene-2-carboxylic acid methyl ester | HCID 57795401 | 76.8% |
反応手順
To a solution of 3-tert-butoxycarbonylamino-5-(1-hydroxy-cyclohexyl)-thiophene-2-carboxylic acid methyl ester (68 g, 0.192 mol) in 400 mL of dichloromethane at 0° C. (ice bath) was added trifluoroacetic acid (400 mL). The mixture was stirred for 30 min at 0° C. and followed by TLC. After completion, the reaction mixture was evaporated to dryness and partitioned between ethyl acetate and saturated water solution of NaHCO3. The organic layer was separated, dried (Na2SO4) and concentrated. The residue was triturated in 4.4 volume of hexane for 30 min. Then filtered and washed with cold hexane. Dried in the vacuum oven to afford 35 g (76%) of 3-Amino-5-cyclohex-1-enyl-thiophene-2-carboxylic acid methyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08674118B2 |
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| 出典データセット | uspto-grants-2014_03 |
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| ORD ID | ord-3c6dfed096ff48cf9186daf7ad0ddd61 |
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| 出典メモ | uspto-grants-2014_03 |
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