化工社化工社 化学情報印刷レポート · 研究参考用
Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- → 1-(3',4'-Dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- | HCID 10036050 | — |
| 反応物 | 1-Iodo-5-(4'-fluorophenyl)-3-pentanone | HCID 20164191 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(3',4'-Dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone | HCID 20164210 | — |
反応手順
To a solution of 48.5 g (0.23 mole) of 2-(3',4'dimethoxyphenyl)-1-nitroethane in 400 ml of dry tetrahydrofuran was added 96.0 (0.23 mole) of 40% Triton B. The solution was stirred at room temperature for 10 minutes. 66.7 g (0.23 mole) of 1-iodo-5-(4'-fluorophenyl)-3-pentanone in a minimum amount of dry tetrahydrofuran was added dropwise. The mixture was heated at 50° C. for 3 hours, then allowed to stir at room temperature overnight. Solvent was removed in vacuo and the residue taken up in ether and extracted twice with water. The organic layer was dried over anh MgSO4, filtered and concentrated at reduced pressure to obtain a crude oil. The crude material was passed through HPLC to give 79 g purified material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04701461 |
| 出典データセット | uspto-grants-1987_10 |
| ORD ID | ord-e02dabff13bf406ab2905c4a71a6a958 |
| 出典メモ | uspto-grants-1987_10 |