참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzyl mercaptan | HCID 7509 | — |
| 반응물 | 2,6-Dibromotoluene | HCID 34681 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | Benzyl(3-bromo-2-methylphenyl)sulfane | HCID 66911186 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08378092B2 |
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| 출처 데이터셋 | uspto-grants-2013_02 |
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| ORD ID | ord-fd0db779b5694582a9c0f17d04f568c4 |
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| 출처 메모 | uspto-grants-2013_02 |
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