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Isobutyryl chloride → Tert-butyl (2-isobutyramido-4-(thiophen-2-yl)phenyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isobutyryl chloride | HCID 62325 | — |
| 反応物 | tert-Butyl (2-amino-4-(thiophen-2-yl)phenyl)carbamate | HCID 57717474 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tert-butyl (2-isobutyramido-4-(thiophen-2-yl)phenyl)carbamate | HCID 71007313 | 81% |
反応手順
To a solution of tert-butyl (2-amino-4-(thiophen-2-yl)phenyl)carbamate (200 mg, 0.689 mmol) in dichloromethane (4 mL) was added isobutyryl chloride (0.08 mL, 0.76 mmol, 1 equiv.) and TEA (0.23 mL, 1.72 mmol, 2.5 equiv.) at 0° C. The reaction was warmed to room temperature and stirred for 16 h. The reaction was then diluted with dichloromethane and water. The organic layers were washed with water and brine, dried over Na2SO4 and concentrated. The crude material was purified by column chromatography (silica gel, EtOAc/hexanes) to afford tert-butyl (2-isobutyramido-4-(thiophen-2-yl)phenyl)carbamate (0.2 g, 81% 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-0b625983cee54cefb2c94de1ba51cf0f |
| 出典メモ | uspto-grants-2016_09 |