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tert-Butyl mercaptan → 3,5-Dichlorophenyl-tert-butylsulfide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butyl mercaptan | HCID 6387 | — |
| 反応物 | 1,3,5-Trichlorobenzene | HCID 7950 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 生成物 | 3,5-Dichlorophenyl-tert-butylsulfide | HCID 18431890 | 19% |
反応手順
To a solution of 4N sodium hydroxide (0.8 ml) was added tert-butylmercaptan (0.406 ml). The mixture was stirred for 15 minutes at room temperature. Tetra n-butylammonium bromide (322 mg, 1 mmol) and 1,3,5-trichlorobenzene (1) (1.8 g, 10 mmol) were added thereto. The reaction mixture was refluxed at 140° C. for 6.5 hours. The reaction mixture was poured into ice-water, extracted with ethylacetate, washed with water, dried over sodium sulphate, filtrated and concentrated under reduced pressure. The obtained residue was chromatographed twice on silica gel (SiO2 15 g, elution: n-hexane) to yield the objective (4) (138 mg). Yield 19%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087764B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-fc08a00bc9a040b3a45a8e40ce7d7458 |
| 出典メモ | uspto-grants-2006_08 |