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Ammonia → HCID 178481735、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | HCID 178515597 | HCID 178515597 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178481735 | HCID 178481735 | 67.2% |
反応手順
30 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1H-pyrazole from Example 3.1 were initially charged in 750 ml of toluene. 23.1 g of dimethyl sulfate and 7.5 g of potassium carbonate were added, and the mixture was heated at reflux for 2 h. After cooling to room temperature, the mixture was made alkaline using ammonia and stirred overnight. The mixture was acidified by addition of hydrochloric acid (pH about 1) and cooled to room temperature, and the precipitated solid was filtered off. Drying gave 21.4 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1-methyl-1H-pyrazole (purity according to GC 99.2%, yield 66.8%). M.p.: 128° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06897322B2 |
| 出典データセット | uspto-grants-2005_05 |
| ORD ID | ord-7699cd7ee4c345c598cec46a2ba68854 |
| 出典メモ | uspto-grants-2005_05 |