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Dimethylcarbamoyl Chloride → Tert-butyl (2-(3,3-dimethylureido)-4-(thiophen-2-yl)phenyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| 反応物 | tert-Butyl (2-amino-4-(thiophen-2-yl)phenyl)carbamate | HCID 57717474 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Tert-butyl (2-(3,3-dimethylureido)-4-(thiophen-2-yl)phenyl)carbamate | HCID 71007375 | 81% |
反応手順
To a solution of tert-butyl 2-amino-4-(thiophen-2yl)phenylcarbamate (0.12 g, 0.41 mmol, 1.0 equiv.) in pyridine (2 mL) was added a solution of dimethylcarbamic chloride (0.07 g, 0.62 mmol, 1.5 equiv.) in toluene (0.3 mL). The resulting solution was stirred at room temperature overnight. The crude residue was diluted with water (10 mL) and extracted with ethyl acetate (10 mL×2). The combined organic layers were washed with water (10 mL), dried, filtered and concentrated. The crude residue was washed with petroleum ether (5 mL) to afford tert-butyl (2-(3,3-dimethylureido)-4-(thiophen-2-yl)phenyl)carbamate (0.12 g, 80% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447030B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-5aa9c5dd39104fa98b5ad0aa30f21e19 |
| 出典メモ | uspto-grants-2016_09 |