化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl isocyanate → [6-(N-Ethylcarbamoyl)-2[4-(N-ethylcarbamoyl)phenyl]benzo[b]thien-3-yl][4-[2-(1-piperidinyl)ethoxy]phenyl]methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl isocyanate | HCID 8022 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Raloxifene Hydrochloride | HCID 54900 | — |
| 反応物 | Isocyanate | HCID 105034 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [6-(N-Ethylcarbamoyl)-2[4-(N-ethylcarbamoyl)phenyl]benzo[b]thien-3-yl][4-[2-(1-piperidinyl)ethoxy]phenyl]methanone | HCID 18357210 | 92.3% |
反応手順
4 g (7.85 mmol) of [6-hydroxy-2-(4-hydroxyphenyl)benzo[b]thien-3-yl][4-[2-(1-piperidinyl)ethoxy]phenyl]methanone hydrochloride was suspended in 250 mL of anhydrous THF and 3 g (30 mmol) of triethylamine was added. The reaction mixture was stirred at room temperature under nitrogen for 15 minutes. 1.67 g (23.5 mmol) of ethylisocyanate was added. After 24 hours, the reaction was checked by TLC, and was not complete. An additional 4.5 g of the isocyanate was added. After 96 hours, the reaction mixture was filtered and chromatographed as in Example 19 to afford 4.23 g of the title compound as a white amorphous powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05482949 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-1c29fa946ec34bdf94ac776a0084de00 |
| 出典メモ | uspto-grants-1996_01 |