化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 3-[1-(4-Methoxyphenyl)-5-(3-pyridyl)-3-pyrazolyl]-propionic acid hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Methoxyphenylhydrazine hydrochloride | HCID 2723904 | — |
| 反応物 | 4,6-Dioxo-6-(3-pyridyl)hexanoic acid | HCID 15169108 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-[1-(4-Methoxyphenyl)-5-(3-pyridyl)-3-pyrazolyl]-propionic acid hydrochloride | HCID 67857336 | 52% |
反応手順
Compound 29 (2.21 g, 10 mM) in methanol (150 ml) containing Et3N (2 ml) was treated with 4-methoxyphenylhydrazine hydrochloride (1.85 g, 10.6 mM) at RT for 4 hr. The solvent was removed in vacuo and the residue was partitioned between 5% NaOH and Et2O. The basic aqueous layer was separated and acidified with 10% HCl to pH 2. Saturated brine was added and the aqueous layer was exhaustively extracted with CH2Cl2. The combined CH2Cl2 layers were concentrated to give the title compound 31 as a tan crystalline solid (Recry. Acetone, 1.87 g, 52%) mp=226°-228° C., MS, m/e 323 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05242940 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-cbbe96bf61684243a07da170a8302318 |
| 出典メモ | uspto-grants-1993_09 |