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4-Methylmorpholine → (S)-3-Methyl-2-[[methyl-(2-pyridinylmethyl)amino]carbonyl]aminobutyric acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Pyridine dihydrochloride | HCID 21954272 | — |
| 反応物 | a-Isocyanato-valine methyl ester | HCID 22845662 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (S)-3-Methyl-2-[[methyl-(2-pyridinylmethyl)amino]carbonyl]aminobutyric acid methyl ester | HCID 10039258 | — |
反応手順
A mixture of 1.61 g (7.2 mmol) of 2-(N-methylamino)methyl)pyridine dihydrochloride and 1.14 g (7.2 retool) of α-isocyanato-valine methyl ester in 40 ml of dichloromethane was treated with 2 ml (18 mmol) of 4-methylmorpholine. After being stirred for 2 h, the solution was partitioned between dichloromethane and water, dried over Na2SO4, and concentrated. Chromatography on silica gel using 2% methanol in chloroform provided 1.94 g (96%) of the desired compound (Rf 0.32, 5% methanol in chloroform) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05461067 |
| 出典データセット | uspto-grants-1995_10 |
| ORD ID | ord-0dc0a455fcb44790871f96243790452c |
| 出典メモ | uspto-grants-1995_10 |