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Acetic Anhydride → 6-Acetoxy-2-{4-[bis(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin | HCID 9804471 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 6-Acetoxy-2-{4-[bis(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin | HCID 19392504 | 92% |
反応手順
Dissolve 0.5 g (1.07 mmol) of the compound obtained in Example 1 at 0° C. in 0.255 ml (2.7 mmol) of acetic anhydride under an inert atmosphere. Add 2 volumes of pyridine (0.5 10 ml) and continue stirring while returning to room temperature for a period of 1 h 30. Neutralise with a saturated sodium hydrogen carbonate solution. After extraction with ether (2×25 ml), the product is purified by chromatography on a silica column (eluant:ethyl acetate/petroleum ether, 20:80) and obtained in pure form as a solid in a yield of 92%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05420132 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-9252ce32aa8042b8a626bae62b7f2fbf |
| 出典メモ | uspto-grants-1995_05 |