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Hexane → 2-[2-(Benzenesulfonyl)-ethylsulfanyl]-3-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 2-Chloro-3-nitropyridine | HCID 79613 | — |
| 反応物 | 2-(Phenylsulfonyl)ethanethiol | HCID 447093 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 2-[2-(Benzenesulfonyl)-ethylsulfanyl]-3-nitropyridine | HCID 67133757 | 46% |
反応手順
1.8 g (16.0 mmol) potassium tert-butylate were added to a solution of 3.0 g (14.8 mmol) 2-(phenylsulfonyl)ethanethiol in DMF (35 ml) and the mixture was stirred for 30 min at room temperature. Then 2.5 g (15.8 mmol) 2-chloro-3-nitropyridine were added and the mixture was stirred for a further 1 h at RT. Then it was diluted with a brine/EE mixture (1:1 vv) and stirred for a further 30 min at RT. Then the organic phase was separated off, washed with water and brine, dried over Na2SO4, filtered and concentrated to small volume under vacuum. Column chromatography (hexane/EE 6:1) of the residue yielded 2.2 g (6.8 mmol, 46%) 2-[2-(benzenesulfonyl)-ethylsulfanyl]-3-nitropyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08247573B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-6cd212b40b0f4f10b0d04144f712bace |
| 出典メモ | uspto-grants-2012_08 |