関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Benzene, 1-bromo-3-nitro- | HCID 11457 | — |
| 反応物 | {4-[(2,3-dihydro-1H-inden-2-ylamino)methyl]-3,5-difluorophenyl}boronic acid | HCID 59316459 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-[(3,5-difluoro-3'-nitro-4-biphenylyl)methyl]-2,3-dihydro-1H-inden-2-amine | HCID 67160310 | — |
反応手順
A mixture of {4-[(2,3-dihydro-1H-inden-2-ylamino)methyl]-3,5-difluoro-phenyl}boronic acid (740 mg, 2.44 mmol; Ex V-22), 3-bromonitrobenzene (495 mg, 2.44 mmol), PdCl2(dppf)2 (100 mg, 0.12 mmol) and Na2CO3 (4.90 mL, 2.0 M (aq)) in DME (10 mL) was stirred at 80° C. for 45 min. The mixture was diluted with EtOAc then filtered through a pad of Celite and silica gel. The filtrate was washed with H2O and brine, dried over Na2SO4 then concentrated to give N-[(3,5-difluoro-3′-nitro-4-biphenylyl)methyl]-2,3-dihydro-1H-inden-2-amine as a tan glass. LC/MS (method A) 0.62 min, (m/z) 381 (70%), 382 (100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822518B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-53a5403519d04d5e939b86c3c3f282f8 |
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| 出典メモ | uspto-grants-2014_09 |
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