化工社化工社 化学情報印刷レポート · 研究参考用
Formic Acid → N-(5-Chloro-2-phenoxy-phenyl)-formamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | 5-Chloro-2-phenoxyaniline | HCID 66738 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(5-Chloro-2-phenoxy-phenyl)-formamide | HCID 12290068 | — |
反応手順
A mixture of 1-amino-5-chloro-2-phenoxybenzene (1.00 g, 4.55 mmol), formic acid (0.34 mL, 9.10 mmol), TBTU (1.46 g, 4.55 mmol), DIEA (2.38 mL, 13.6 mmol) and DCM (20 mL) was stirred at rt for 2 h. The solution was transferred to a separatory funnel, 20 mL of sat. aq. NaHCO3 solution was added and the mixture was extracted DCM. The organics were combined and dried (Na2SO4). Solvent was removed under reduced pressure to give a crude residue which was purified via flash chromatography, eluting with 5% EtOAc in hexanes.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08481733B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-e8058ec2bec9481493262bcce1b83675 |
| 出典メモ | uspto-grants-2013_07 |