참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | (e)-(2-Chlorobenzylidene)hydrazine | HCID 9629214 | — |
| 반응물 | 2,4-Dichloro-6-methylpyridine | HCID 11959083 | — |
| 촉매 | CID 53485975 | HCID 53485975 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | HCID 59261367 | HCID 59261367 | 31.4% |
반응 단계
(E)-1-(2-chlorobenzylidene)hydrazine (0.351 g, 2.27 mmol), dichloro[1,1′bis(diphenylphosphino)ferrocene]palladium (II) dichloromethane adduct (0.0185 g, 0.0227 mmol) and potassium carbonate (0.471 g, 3.41 mmol) was added to a 50-mL RBF. Toluene (2 mL) was added and 2,4-dichloro-6-methylpyridine (0.368 g, 2.27 mmol) in 3 mL of toluene was added. The red mixture was heated to 100° C. After 18 h, the reaction was allowed to cool to RT and water (20 mL) was added. The mixture was filtered and 190 mg of (E)-1-(2-chlorobenzylidene)-2-(4-chloro-6-methylpyridin-2-yl) hydrazine was collected as a tan solid. The filtrate was absorbed on silica gel and purified by silica gel chromatography (8/2 hexanes/DCM to 7/2/1 hexans/DCM/EtOAc) to afford an additional 200 mg of (E)-1-(2-chlorobenzylidene)-2-(4-chloro-6-methylpyridin-2-yl) hydrazine as a tan solid. MS (ESI, pos. ion) m/z: 280.0 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07700593B2 |
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| 출처 데이터셋 | uspto-grants-2010_04 |
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| ORD ID | ord-18f87604d6eb4ec6913459692f7693df |
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| 출처 메모 | uspto-grants-2010_04 |
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