関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 2-Chloro-5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)nicotinonitrile | HCID 10150677 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-(2,4-Dichlorophenyl)-5-(4-chlorophenyl)-2-(methylamino)pyridine-3-carbonitrile | HCID 68719045 | — |
反応手順
To 2-chloro-6-(2,4-dichlorophenyl)-5-(4-chlorophenyl)pyridine-3-carbonitrile (2.03 g) in THF (14 mL) was added H2NCH3 (13 mL, 2 M solution in THF). The reaction was heated to 67° C. in a closed vessel for 9 hours before concentrating. The product was dissolved in EtOAc and washed with saturated aqueous NaHCO3 solution. The solution was concentrated and purified via flash chromatography on silica gel with a gradient elution of 0% to 10% EtOAc in hexane affording the title compound. HPLC/MS: 387.8(M+1), 389.8 (M+3); Rt=4.26 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728141B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-8388cc3948c24d1aa622a1a5a14c0e04 |
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| 出典メモ | uspto-grants-2010_06 |
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