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Methanol → E-4031 dihydrochloride
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 | N-[4-(piperidine-4-carbonyl)-phenyl]methanesulfonamide hydrochloride | HCID 14130042 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | E-4031 dihydrochloride | HCID 3087190 | 150.7% |
反応手順
0.254 g (0.797 mmol) of 4-(4-methylsulfonylaminobenzoyl)piperidine hydrochloride, 0.22 g (1.88 mmol) of 6-methyl-2-vinylpyridine and 0.15 g of sodium acetate were suspended in 3 ml of a mixture of methanol and water (1:1) and the suspension was refluxed for 2 h. The liquid reaction mixture was filtered and the filtrate was concentrated. The obtained residue was purified according to silica gel column chromatography (chloroform:methanol:aqueous ammonia=96:4:0.4). The purified product was converted into its hydrochloride with ethanolic hydrogen chloride and recrystallized from ethanol to obtain 0.285 g (yield: 81%) of the intended compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05118689 |
| 出典データセット | uspto-grants-1992_06 |
| ORD ID | ord-50e352dc85014b8fa31de93c71520f74 |
| 出典メモ | uspto-grants-1992_06 |