関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (S)-2-(Boc-Amino)-N-methoxy-n-methylbutyramide | HCID 10422029 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | tert-butyl N-((2S)-1-oxobutan-2-yl)carbamate | HCID 10241556 | — |
反応手順
To a solution of LiAlH4 (0.453 g, 11.9 mmol) in Et2O (20 mL) at 0° C. was added dropwise a solution of 1,1-dimethylethyl ((1S)-1-{[methyl(methyloxy)amino]carbonyl}-propyl)carbamate (2.67 g, 10.8 mmol) in Et2O (15 mL). The reaction mixture was stirred for 30 min at 0° C. and quenched with EtOAc (6.5 mL) followed by 5% aq. potassium bisulfate (6.5 mL). The reaction mixture was washed with 1 M aq. HCl (3×10 mL), saturated aq. NaHCO3 (3×10 mL), and brine (10 mL). The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo to afford the title compound as a clear, colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841463B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-5760667bccfa440ab1833c283b8e4596 |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|