関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-BOC-ethylenediamine | HCID 187201 | — |
| 反応物 | 3-Fluoro-4-nitroanisole | HCID 565654 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | tert-Butyl (2-((5-methoxy-2-nitrophenyl)amino)ethyl)carbamate | HCID 59345555 | 104% |
反応手順
A 2 L flask equipped with a stir bar was charged with DMSO (800 mL), K2CO3 (161 g, 1.6 mol) and 4-methoxy-2-fluoro-1-nitrobenzene (10 g, 0.58 mol). Mono-N-Boc-1,2-diaminoethane (94 g, 0.55 mol) was added to the reaction mixture and stirred for 12 h at 60° C. The reaction mixture was triturated with ice cold water (1.2 L) and the resulting yellow precipitate was collected by vacuum filtration. The precipitate washed several times with water (5×1 L) and dried on a high vacuum for 48 h to give the desired product as a bright yellow solid (178 g, 98%.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741355B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-da35237a06ea4009a1592d9924c75584 |
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| 出典メモ | uspto-grants-2010_06 |
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