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Water → 2-(1-(3-(Trifluoromethyl)phenyl)ethylidene)hydrazinecarboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Hydrazinecarboxylic acid, ethyl ester | HCID 20064 | — |
| 反応物 | 3'-(Trifluoromethyl)acetophenone | HCID 67682 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(1-(3-(Trifluoromethyl)phenyl)ethylidene)hydrazinecarboxylic acid ethyl ester | HCID 54412625 | 100% |
反応手順
m-Trifluoromethylacetophenone (74 g, 0.394 mole), ethyl carbazate (43 g, 0.413 mole), and catalytic p-toluenesulfonic acid (20 mg) were refluxed under N2 over a Dean-Stark trap in toluene (1.2 L) until the theoretical amount of water of reaction was removed (7.1 mL, 6 h). The solvent was then removed in vacuo and 2-(1-(3-(trifluoromethyl)phenyl)ethylidene)hydrazinecarboxylic acid ethyl ester (107 g, 100% yield) was obtained as a white solid which was recrystallized from cyclohexane, mp=94°-96° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05623072 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-ccecdd3cd98e4bafa7a846607a35e3de |
| 出典メモ | uspto-grants-1997_04 |