関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-((((Benzyloxy)carbonyl)amino)methyl)benzoic acid | HCID 1479997 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | (2S)-2-amino-5-(((tert-butoxy)carbonyl)amino)pentanoic acid | HCID 6993436 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | HCID 86592268 | HCID 86592268 | 38% |
反応手順
The compound obtained in Example 23-2 (350 mg) was dissolved in DMF (7 ml). After the addition of WSCI hydrochloride (265.0 g), DMAP (169 mg), and the compound obtained in Example 41-1 (276.0 mg), the mixture was stirred for 24 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was dissolved in chloroform, washed with 1 mol/l aqueous solution of hydrochloric acid and saturated aqueous solution of sodium hydrogencarbonate, and dried over sodium hydrogensulfate. The solvent was removed by distillation and the residue was purified by silica gel column chromatography (20 g, chloroform/methanol=10/1). 130 mg of the obtained product was dissolved in methanol (2.6 ml) and 4 mol/l hydrochloric acid/dioxane solution (2.6 ml) was added. The mixture was stirred for 70 minutes at room temperature. After the reaction, the solvent was removed by distillation and the residue was dried under vacuum to obtain hydrochloride of the title compound (147 mg) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07098215B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-447f2211d39544d9a51ee1929e302857 |
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| 出典メモ | uspto-grants-2006_08 |
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