化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Iodide → 3-(4-Methoxybenzyloxycarbonyl)-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Methyloxybenzyl chloride | HCID 69993 | — |
| 反応物 | 3-Carboxy-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran | HCID 19795843 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3-(4-Methoxybenzyloxycarbonyl)-2-methylthio-4-oxo-6,7,8-trifluoro-4H-1-benzothiopyran | HCID 54528214 | 32.4% |
反応手順
To a suspension of 50 mg (0.163 mmol) of the compound of Example 112 in 0.2 ml of chloroform were added 30.7 mg (0.196 mmol) of p-methoxybenzyl chloride, 16.5 mg (0.163 mmol) of triethylamine and 29.4 mg (0.196 mmol) of sodium iodide, and the mixture was stirred for 5 hours at room temperature, which was poured into ice-water and extracted with dichloromethane. The organic layer was washed with water and with saturated saline solution, dried over anhydrous sodium sulfate and concentrated. The residue was purified by means of silica gel column chromatography (CHCl3) to obtain 22.5 mg (0.0528 mmol) of title compound (yield 32%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05244892 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-650824152b5742c386e87f846affa28e |
| 出典メモ | uspto-grants-1993_09 |