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tert-Butyl hydrogen {2-[benzyl(methyl)amino]ethyl}carbonimidate → N-(tert-Butoxycarbonyl)-N'-methylethylenediamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butyl hydrogen {2-[benzyl(methyl)amino]ethyl}carbonimidate | HCID 50999034 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-(tert-Butoxycarbonyl)-N'-methylethylenediamine | HCID 3435744 | 68.3% |
反応手順
A mixture of tert-butyl 2-(benzyl(methyl)amino)ethylcarbamate (1.20 g, 4.54 mmol), 10% Pd/C (0.90 g) and MeOH (60 mL) was stirred under a H2 atmosphere (0.8 MPa, RT, 16 h). The mixture was filtered and concentrated under reduced pressure. The crude material was purified by column chromatography on silica gel, eluting with saturated N3 in MeOH-DCM (0-10%) to afford tert-butyl 2-(methylamino)ethylcarbamate as a colorless oil (0.54 g, 68.3%). 1HNMR (CDCl3): δ 3.25 (m, 2H, CH2), 2.7 (m, 2H, CH2), 2.49 (s, 3H, CH3), 1.49 (s, 9H, CH3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846972B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-7f94609dbdc24017a2276af309511796 |
| 出典メモ | uspto-grants-2014_09 |