関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Methyl phenyl sulfone | HCID 18369 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl (1-cyclopentylethylamino)benzoate | HCID 54103355 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 4'-(1-Cyclopentylethylamino)-2-(phenylsulfonyl)acetophenone | HCID 20499012 | — |
反応手順
A solution of 864 mg. of sodium hydride and 5.3 g. of methylphenylsulfone in 20 ml. of 1,2-dimethoxyethane is stirred at 6° C. for one hour under an atmosphere of argon. To this solution is added a solution of 5.0 g. of methyl (1-cyclopentylethylamino)benzoate in 50 ml. of tetrahydrofuran and the reaction mixture is stirred at 60° C. for 1.5 hours. The mixture is cooled, poured onto ice, acidified with dilute hydrochloric acid and pH 3 and then extracted with chloroform. The organic layer is separated, washed with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate and then concentrated to dryness. The crude solid is chromatographed on silica gel, eluting with methylene chloride to yield 4'-(1cyclopentylethylamino)-2-(phenylsulfonyl)acetophenone.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04259352 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-5d91c82e3b2d43059a90c136a85010c3 |
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| 出典メモ | uspto-grants-1981_03 |
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