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Lithium Hydroxide → N-((N-Methyl-N-((2-pyridinyl)methyl)amino)carbonyl)valine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | (S)-3-Methyl-2-[[methyl-(2-pyridinylmethyl)amino]carbonyl]aminobutyric acid methyl ester | HCID 10039258 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N-((N-Methyl-N-((2-pyridinyl)methyl)amino)carbonyl)valine | HCID 10106914 | 85% |
反応手順
A solution of 4.47 g (16 mmol) of N-((N-methyl-N-((2-pyridinyl)methyl)-amino)carbonyl)valine methyl ester in 65 ml of dioxane was treated with 65 ml of 0.5 M aqueous lithium hydroxide. After being stirred at ambient temperature for 1 h, the resulting solution was concentrated in vacuo to a small volume (ca. 5 ml), neutralized to pH 5 with 1 M aqueous HCl, and extracted with three 100 ml portions of ethyl acetate. The combined organic layers were dried over Na2SO4 and concentrated in vacuo to provide 3.61 g (85%) of the desired compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05990135 |
| 出典データセット | uspto-grants-1999_11 |
| ORD ID | ord-d7c1361db56341af9b14c9f42df88b2a |
| 出典メモ | uspto-grants-1999_11 |