関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2,2'-Dipyridylamine | HCID 14547 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl 6-Bromohexanoate | HCID 4170292 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 6-(Di-pyridin-2-yl-amino)-hexanoic acid methyl ester | HCID 58545021 | 24% |
反応手順
NaH (112 mg, 2.92 mmol) was added to di-pyridin-2-yl-amine (500 mg, 2.92 mmol) in DMF (10 mL) at rt. After 10 min, KI (485 mg, 2.92 mmol) and methyl 6-bromohexanoate, I (0.464 mL, 2.92 mmol) were added, and the reaction mixture was stirred at 90° C. for 21 h. Brine (200 mL) and EtOAc (200 mL) were then added, the phases were separated, and the aqueous phase was extracted with EtOAc (100 mL). The organic phases were combined, dried over MgSO4, filtered, and subsequently evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using CH2Cl2/MeOH (100:0.5 to 100:1) as eluant to furnish II as a colourless oil (206 mg, 24%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08748458B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-9a11980996a44e3fa56ecda51bb47bfd |
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| 出典メモ | uspto-grants-2014_06 |
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