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Methanol → 1-[2-(6-Methyl-2-pyridyl)ethyl]-4-(4-methylsulfonylaminophenylsulfonyl)piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 2-Ethenyl-6-methylpyridine | HCID 70735 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 4-(4-Methylsulfonylaminophenylsulfonyl)piperidine hydrochloride | HCID 18539239 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[2-(6-Methyl-2-pyridyl)ethyl]-4-(4-methylsulfonylaminophenylsulfonyl)piperidine | HCID 15027722 | 64% |
反応手順
0.60 g (1.86 mmol) of 4-(4-methylsulfonylaminophenylsulfonyl)piperidine hydrochloride obtained in Example 5, 0.44 g (3.72 mmol) of 6-methyl-2-vinylpyridine and 0.31 g of sodium acetate were suspended in 10 ml of a mixture of methanol with water (1:1) and the suspension was refluxed for 2 h. The reaction liquid was filtered and the filtrate was concentrated to give a residue. After extraction with dichloromethane followed by washing with water, the organic layer was concentrated to precipitate white crystals. The crystals were collected by filtration and recrystallized from ethyl acetate to give 0.52 g (yield: 64%) of the intended compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05162347 |
| 出典データセット | uspto-grants-1992_11 |
| ORD ID | ord-e55315fc54894454a029f58dd9684473 |
| 出典メモ | uspto-grants-1992_11 |