化工社化工社 化学情報印刷レポート · 研究参考用
Benzaldehyde → HCID 178469930、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzaldehyde | HCID 240 | — |
| 反応物 | HCID 178469928 | HCID 178469928 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178469930 | HCID 178469930 | — |
反応手順
21.2 g of benzaldehyde is added to a suspension of 25 g of 3-amino-4-ethoxycarbonylpyrazole in 200 ml of toluene. The whole is boiled while separating water. In 3 hours a total of 5 ml of water collects. After the toluene has been evaporated, 50 ml of methanol and 50 ml of THF are added and, under cooling, 23 g of NaBH4 is added at 0°-5° C. After 4 hours' at room temperature, the solvent mixture is drawn off; then 200 ml of ice water is added the whole is extracted three times with 150 ml of methylene chloride each time and the extract is dried over Na2SO4. After concentration, an oil remains that is recrystallized from ligroin/toluene; m.p. 99°-100° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04354031 |
| 出典データセット | uspto-grants-1982_10 |
| ORD ID | ord-2ec90a6fb4714466a6ec45db3520de38 |
| 出典メモ | uspto-grants-1982_10 |