참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 2,2'-Dipyridylamine | HCID 14547 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Methyl 6-Bromohexanoate | HCID 4170292 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | 6-(Di-pyridin-2-yl-amino)-hexanoic acid methyl ester | HCID 58545021 | 24% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08748458B2 |
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| 출처 데이터셋 | uspto-grants-2014_06 |
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| ORD ID | ord-9a11980996a44e3fa56ecda51bb47bfd |
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| 출처 메모 | uspto-grants-2014_06 |
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