化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 2H-Benzotriazole, 2-phenyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Iodo benzene diacetate | HCID 12217721 | — |
| 反応物 | HCID 178420498 | HCID 178420498 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2H-Benzotriazole, 2-phenyl- | HCID 154096 | 34% |
反応手順
2-phenylazoaniline (3.47 g, 17.6 mmol) prepared above was placed in a 100-mL 1-neck round bottomed flask. Acetic acid (20 mL) and iodobenzene diacetate (6.23 g, 19.4 mmol) were added, in that order, resulting in an exotherm. The reaction was allowed to proceed for 1 hour during which time the mixture cooled to room temperature. Dichloromethane and water were added to the reaction mixture. The organic layer was separated and dried over MgSO4. The solution was filtered and concentrated using a rotary evaporator. The residue was purified on a silica gel column using dichloromethane as eluent. The fractions containing the desired product were combined and solvent removed. The solid was dried in a vacuum oven for 2 h. Yield: 34%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07714099B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-a3dae15437e442f885108eed9e767164 |
| 出典メモ | uspto-grants-2010_05 |