関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 反応物 | 4-[Cyclohexyl-(2-ethoxycarbonyl-ethyl)-amino]-2-methylsulfanyl-pyrimidine-5-carboxylic acid ethyl ester | HCID 68583496 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | HCID 68583787 | HCID 68583787 | 63% |
反応手順
Sodium (25 wt % dispersion in paraffin wax, 0.10 g, 3.8 mmol) was added to t-butanol (1.8 mL) at rt. After 10 minutes, a solution of 4-[cyclohexyl-(2-ethoxycarbonyl-ethyl)-amino]-2-methylsulfanyl-pyrimidine-5-carboxylic acid ethyl ester (1.0 g, 2.5 mmol) in 10 mL of toluene was added to the sodium t-butoxide solution and the resulting mixture was heated at 90° C. for 30 minutes. The reaction mixture was then cooled and the solution was adjusted to pH 7 using a 1N HCl solution. The solution was then extracted with EtOAc (2×20 mL) and the organic layer was dried (MgSO4) and concentrated to provide 0.55 g (42%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728003B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-41677c4f3045402cbb69067e5b147a3b |
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| 出典メモ | uspto-grants-2010_06 |
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