化工社化工社 化学情報印刷レポート · 研究参考用
Aniline → 3-Aminobenzanilide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-Aminobenzoic acid hydrochloride | HCID 3084218 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Aminobenzanilide | HCID 84347 | 34.4% |
反応手順
HATU (230 mg, 0.605 mmol) and aniline (0.063 mL, 0.691 mmol) was added to a solution of 3-aminobenzoic acid hydrochloride (100 mg, 0.576 mmol) and N,N-diisopropylethylamine (0.217 mL, 1.267 mmol) in 1.5 mL of DMF. The reaction solution was stirred at RT for 3 h. The crude material was purified by reverse-phase preparative HPLC using 0.1% TFA in CH3CN/H2O, gradient 20% to 45%. Desired fractions were collected and the solvents were removed under reduced pressure. The residue was passed through 2 g SCX column and washed by 2M NH3 in MeOH to provide 3-amino-N-phenylbenzamide (42 mg, 0.198 mmol, 34.4% yield) as a light-yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09334269B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-1bf81f3be6c445a1a476271b1692c707 |
| 出典メモ | uspto-grants-2016_05 |