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Methanamine, N-methoxy-, hydrochloride (1:1) → tert-Butyl N-{1-[methoxy(methyl)carbamoyl]propyl}carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-(((Tert-butoxy)carbonyl)amino)butanoic acid | HCID 333522 | — |
| 反応物 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | tert-Butyl N-{1-[methoxy(methyl)carbamoyl]propyl}carbamate | HCID 19364648 | 63% |
反応手順
2-tert-Butoxycarbonylamino-butyric acid (500 mg, 2.46 mmol), HBTU (1.03 g, 2.71 mmol) and DIPEA (1.22 mL, 7.38 mmol) were dissolved in DMF (10 mL) and stirred for 30 min. N,O-dimethylhydroxylamine hydrochloride (360 mg, 3.69 mmol) was added and the reaction mixture was stirred for 1 h. The solvents were removed in vacuo and the residue was purified by column chromatography to give the title compound (380 mg, 63%) as a cream oil. LCMS (ES+): 269.2 [MNa]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09353086B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-0d45fff0f88f44cd81d07c8ba792f92b |
| 出典メモ | uspto-grants-2016_05 |