関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| 反応物 | HCID 22567500 | HCID 22567500 | — |
| 反応物 | 3-(1-hydrazonoethyl)-1-methyl-5-[4-(trifluoromethyl)phenyl]-1H-pyrazol-4-ol | HCID 72360113 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 73299960 | HCID 73299960 | 100% |
反応手順
3-Amino-N-(2-carbamoylethyl)benzamide (56 mg, 0.27 mmol) was stirred with a dimethylformamide solution of thiocarbonyldiimidazole (0.1 M, 2.25 mL, 0.225 mmol) at room temperature for 1.5 hours, and then with a dimethylformamide solution of 3-(1-hydrazonoethyl)-1-methyl-5-[4-(trifluoromethyl)phenyl]-1H-pyrazol-4-ol prepared in Reference Synthetic Example 14 (0.1 M, 1.8 mL, 0.18 mmol) at 40° C. for 1 hour, and then stirred at room temperature for 17 hours. After addition of water and saturated aqueous sodium chlorides the solution was extracted with ethyl acetate, and the extract was dried over anhydrous sodium sulfate and filtered. The solvent was evaporated, and chloroform and hexane were added to the residue. The precipitated solid was collected by filtration, washed with hexane and dried to give 102.7 mg of the desired product (yield 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08134013B2 |
|---|
| 出典データセット | uspto-grants-2012_03 |
|---|
| ORD ID | ord-04b6e6d46024437f8a2a135594c1ee36 |
|---|
| 出典メモ | uspto-grants-2012_03 |
|---|