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2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine → 3,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-(p-tolylsulfonyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine | HCID 19935587 | — |
| 反応物 | Sodium 4-methylbenzene-1-sulfinate--water (1/1/4) | HCID 23690860 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-(p-tolylsulfonyl)pyridine | HCID 19935608 | 57.9% |
反応手順
A mixture of 0.379 g of 2-chloro-3,4- diethoxycarbonyl-5-nitro-6-phenylpyridine, 0.5 g of sodium p-toluenesulfinate tetrahydrate and 15 ml of ethanol was heated under reflux for 3 hours. After concentration, the concentrate was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride, and dried over sodium sulfate. After the solvent was distilled off, the residue was subjected to silica gel column chromatography with n-hexane/ethyl acetate (4:1) as the eluent. The eluate was concentrated to give crystals. The obtained crystals were recrystallized from the same solvent, to give 0.289 g of the title compound as colorless needles.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05420275 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-e8df5648462847aea31600732ea0cdf2 |
| 出典メモ | uspto-grants-1995_05 |