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Acetic Acid → tert-Butyl 4-sulfanylpiperidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | tert-Butyl 4-(acetylthio)piperidine-1-carboxylate | HCID 22494773 | — |
| 反応物 | Sodium methanolate methanol | HCID 23694274 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | tert-Butyl 4-sulfanylpiperidine-1-carboxylate | HCID 21906090 | 98.9% |
反応手順
In dry methanol were dissolved 520 mg (2 mmol) of 4-(acetylthio)-1-(tert-butoxycarbonyl)piperidine, and 420 μl (2 mmol) of a 28% sodium methoxide-methanol solution were added to the mixture under ice-cooling and under a nitrogen atmosphere, followed by stirring of the resulting mixture for 40 minutes. Then, 173 μl of acetic acid were added to the mixture and the solvent was distilled off at room temperature, followed by diluting of the residue with ethyl acetate. The mixture was washed successively with an aqueous sodium hydrogencarbonate solution and an aqueous NaCl solution in the order and the solvent was distilled off to obtain 430 mg of reddish orange oil. This product was used for a subsequent reaction without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06300357B1 |
| 出典データセット | uspto-grants-2001_10 |
| ORD ID | ord-6e02e78c80f640369042e7db9c28b062 |
| 出典メモ | uspto-grants-2001_10 |