関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Acetaldehyde, bromo- | HCID 105131 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 1-Methylpiperidine-4-thiol | HCID 14180391 | — |
| 生成物 | 4-[(2,2-Diethoxyethyl)thio]-1-methylpiperidine | HCID 19936607 | — |
反応手順
Sodium methylate (18.1 g) is added in portions to a solution of 1-methylpiperidine-4-thiol (22 g) in anhydrous tetrahydrofuran (200 ml). After one hour, the diethyl acetal of bromoacetaldehyde (30.3 ml) is added. After 4 hours at room temperature, the solution is heated for 2 hours at 40° C. The insoluble material is filtered off and rinsed with THF. The filtrate is concentrated and then distilled under reduced pressure to give 4-[(2,2-diethoxyethyl)thio]-1-methylpiperidine (36 g; b.p.=104°-108° C. under 0.05 atm) in the form of an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05418242 |
|---|
| 出典データセット | uspto-grants-1995_05 |
|---|
| ORD ID | ord-0036740931ac42919ebbc0deb994d2c7 |
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| 出典メモ | uspto-grants-1995_05 |
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