関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 3,3,3-Trifluoropropionic acid | HCID 2777972 | — |
| 反応物 | 2-((Tert-butyldimethylsilyloxy)methyl)-4-methoxyaniline | HCID 66980081 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-((tert-butyldimethylsilyloxy)methyl)-4-methoxyphenyl)-3,3,3-trifluoropropanamide | HCID 66980120 | — |
反応手順
A mixture of 2-((tert-butyldimethylsilyloxy) methyl)-4-methoxyaniline (14.0 g), 3,3,3-trifluoro-propionic acid (7.30 g, 57.0 mmol), EDCI (15.0 g, 76.5 mmol), HOBT (11.0 g, 80.2 mmol) and NMM (22 mL, 157 mmol) in anhydrous CH2Cl2 (200 mL) was stirred at 20° C. for 2 hours. The mixture was diluted with CH2Cl2 (100 mL), the organic layer was washed with 1M HCl (100 mL), H2O (100 mL) and brine (100 mL), dried over Na2SO4 and concentrated to give the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09433618B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-773b12b6404c462f850499a2e177f047 |
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| 出典メモ | uspto-grants-2016_09 |
|---|
