関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 5-Cyclohex-1-enyl-3-[(3-oxo-octahydro-indolizin-7-yl)-amino]-thiophene-2-carboxylic acid methyl ester | HCID 57795496 | — |
| 反応物 | HCID 178461265 | HCID 178461265 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178499270 | HCID 178499270 | 64% |
反応手順
trans-4-Methylcyclohexyl carboxylic acid chloride was added to a solution of 5-cyclohex-1-enyl-3-[(3-oxo-octahydro-indolizin-7-yl)-amino]-thiophene-2-carboxylic acid methyl ester (698 mg, 1.86 mmol) and pyridine (166 μL, 2.05 mmol) in dry toluene (8 mL). The mixture was refluxed for 16 h, then it was brought to room temperature, additional amount of pyridine (0.2 mL) and MeOH (1 mL) were added. The mixture was diluted with dichloromethane, washed with brine; organic phase was dried over Na2SO4, concentrated and purified by column chromatography on silica gel using gradient 0-100% EtOAc in hexane to afford 592 mg (64%) of 5-cyclohex-1-enyl-3-[(trans-4-methyl-cyclohexanecarbonyl)-(3-oxo-octahydro-indolizin-7-yl)-amino]-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 | US07569600B2 |
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| 出典データセット | uspto-grants-2009_08 |
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| ORD ID | ord-1a681a0c12ef4c1c95be08b6c592dc9d |
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| 出典メモ | uspto-grants-2009_08 |
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