참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Amino-4-chloropyridine | HCID 581866 | — |
| 반응물 | 5-Cyclopropylnicotinonitrile | HCID 57419623 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178512052 | HCID 178512052 | — |
반응 단계
n-Butyllithium (1.6 M, 2.2 mL, 0.0034 mol) was added slowly for a period of 5 min to a solution of 4-chloropyridin-2-amine (0.4 g, 0.0031 mol) in anhydrous tetrahydrofuran (20 mL) at −78° C. The reaction temperature was raised to −40° C. and stirred for 15 min. The reaction mixture was cooled to −78° C. and 5-cyclopropylnicotinonitrile (0.45 g, 0.0031 mol) in tetrahydrofuran (5 mL) was added. The temperature was raised to RT and stirred it for 3 h. The reaction mixture was quenched with a saturated aqueous ammonium chloride solution (25 mL) then extracted with ethyl acetate (2×50 mL). The combined organic layers were dried over sodium sulphate and concentrated under vacuum to afford the crude product, which was recrystalised with a DCM and ether mixture to afford the title compound. MS (M−1): 271.0.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09193724B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-d8c3e655819a4365bb6868c4d24a8396 |
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| 출처 메모 | uspto-grants-2015_11 |
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