化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → HCID 178491357、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2-Bromo-4'-(trifluoromethyl)acetophenone | HCID 321979 | — |
| 反応物 | HCID 178491371 | HCID 178491371 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 178491357 | HCID 178491357 | 52.9% |
反応手順
Preparation took place analogously to Example 3 by reaction of 140 mg (0.52 mmol) N-[[(2,6-dimethoxybenzyl)amino](imino)methyl]thiourea with 140 mg (0.52 mmol) 4-(trifluoromethyl)phenacyl bromide. The educts were suspended in 3 ml dioxane, were added to 0.3 ml acetic acid and were heated for 40 minutes in the microwave (radiation 300 Watt). The mixture was subsequently concentrated and the crude product obtained was purified by chromatography on silica gel (dichloromethane/methanol 1-4%). Stirring of the yellow foam obtained with methyl tert.-butyl ether yielded 120 mg of a white amorphous solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08431604B2 |
| 出典データセット | uspto-grants-2013_04 |
| ORD ID | ord-18bb78271e744dd0b06c3577ed06103e |
| 出典メモ | uspto-grants-2013_04 |