関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl mercaptan | HCID 7509 | — |
| 反応物 | 2,6-Dibromotoluene | HCID 34681 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Benzyl(3-bromo-2-methylphenyl)sulfane | HCID 66911186 | — |
反応手順
2,6-dibromotoluene (20 g, 100 mmol) in dioxane (160 ml) was stirred under argon. Then, DIPEA (30.9 ml, 160 mmol), xantphos (2.77 g, 4.8 mmol) and Pd2(dba)3 (2.4 g, 2.4 mmol) were added and the reaction was heated to 100° C. Phenyl-methanethiol (9.4 ml, 80 mmol) was slowly added and the reaction stirred for 6 h. The reaction was quenched by the addition of 150 ml of H2O. After extraction (three times) with ethyl acetate, the combined organic layers were washed with water, dried with Na2SO4, evaporated to dryness and the product was purified by silica gel chromatography.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08378092B2 |
|---|
| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-fd0db779b5694582a9c0f17d04f568c4 |
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| 出典メモ | uspto-grants-2013_02 |
|---|
