関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | ((2-Chloroethyl)thio)benzene | HCID 21702 | — |
| 反応物 | HCID 178526679 | HCID 178526679 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Nitro-2-(2-phenylsulfanyl-ethylsulfanyl)pyridine | HCID 67134239 | 66% |
反応手順
3.44 g (20.0 mmol) (2-chloroethyl)(phenyl)sulfane and 5.53 g (40.0 mmol) potassium carbonate were added to a solution of 1.56 g (10.0 mmol) 2-mercapto-3-nitropyridine in DMF (30 ml) and heated for 4 h at 60° C. Then the mixture was diluted with EE and washed with brine. The organic phase was separated off, dried over Na2SO4, filtered and concentrated to small volume under vacuum. Column chromatography (hexane/EE 9:1) of the residue yielded 1.93 g (6.6 mmol, 66%) 3-nitro-2-(2-phenylsulfanyl-ethylsulfanyl)pyridine.
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 |
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| ORD ID | ord-d3e7cedc03e24bf9af5227f9c7d87216 |
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| 出典メモ | uspto-grants-2012_08 |
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