참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-Chloro-6-methylpyridazine | HCID 227254 | — |
| 반응물 | 2-Dibenzothiophenamine | HCID 298442 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-(6-Methylpyridazin-3-ylamino)dibenzothiophene | HCID 22277796 | 34.7% |
반응 단계
A mixture of 2-aminodibenzothiophene (0.90 g, 4.52 mM), 3-chloro-6-methyl-pyridazine (0.58 g, 4.52 mM), sodium t-butoxide (0.61 g, 6.33 mM), tris(dibenzylidene-acetone)dipalladium(0) (0.083 g, 0.09 mM) and S-2,2′-bis(diphenylphosphino)-1,1′-binapthyl (0.113 g, 0.18 mM) in toluene (23 ml) was heated to 80° C. for 18 hours under an inert atmosphere. On cooling to room temperature the mixture was diluted with DCM, washed with aqueous potassium carbonate, dried over sodium sulphate and concentrated. Chromatography (eluent gradient of DCM to EtOAc then MeOH:EtOAc (1:9)) gave the product as an off white solid (0.456 g). NMR: 9.38 (brs, 1H), 8.81 (brs, 1H), 8.18 (m, 1H), 8.01 (m, 1H), 7.94 (d, 1H), 7.75 (dd, 1H), 7.50 (m, 1H), 7.36 (d, 1H), 7.14 (d, 1H), 2.50 (s, 3H); m/z 292.29.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06967216B2 |
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| 출처 데이터셋 | uspto-grants-2005_11 |
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| ORD ID | ord-9559bbad7a0d43079c2afd368f2ac88f |
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| 출처 메모 | uspto-grants-2005_11 |
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