関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 1-(Trimethylsilyl)ethanol | HCID 12447898 | — |
| 反応物 | 4-((5,6,7,8-Tetrahydro-8,8-dimethyl-5-oxonaphth-2-yl)ethynyl]benzoic acid | HCID 15345547 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (Trimethylsilyl)ethyl 4-[(5,6,7,8-tetrahydro-8,8-dimethyl-5-oxonaphth-2-yl)ethynyl]benzoate | HCID 54412444 | — |
反応手順
To a solution of 0.24 g (0.73 mmol) of 4-[(5,6,7,8-tetrahydro-8,8-dimethyl-5-oxonaphth-2-yl)ethynyl]benzoic acid (Compound 7) in 10 ml of dry CH2Cl2 was added 0.09 g (0.74 mmol) of dimethylaminopyridine, 0.115 ml (0.80 mmol) of trimethylsilylethanol and 0.17 g (0.88 mmol) of 1-(3-dimethylaminopropyl)-3-ethyl carbodiimide hydrochloride. The reaction mixture was stirred at 25° C. for 5 hours, washed with sat. aqueous NaHCO3 and brine, dried over Na2SO4 and concentrated in vacuo to an oil. Purification by flash chromatography (silica, 10% EtOAc-hexane) yielded the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05723620 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-558960f60108438697a2928369019551 |
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| 出典メモ | uspto-grants-1998_03 |
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