참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1-(3-Pyridyl)-3-(dimethylamino)-2-propen-1-one | HCID 567033 | — |
| 반응물 | HCID 178459007 | HCID 178459007 | — |
| 용매 | 1-Butanol | HCID 263 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 68573992 | HCID 68573992 | — |
반응 단계
A stirred mixture of {2-[(2-propenyloxy)-methyl]-5-nitro-phenyl}-guanidine (3.75 g, 15 mmol), 3-(dimethylamino)-1-(3-pyridinyl)-2-propen-1-one (2.60 g, 15 mmol) and ethyl diisopropylamine (2.6 mL, 15 mmol) in 1-butanol (50 mL) is heated at 120° C. for 20 h. The solvent is then evaporated off under reduced pressure to give a residue which is dissolved in ethyl acetate (100 mL). The resulting mixture is filtered (celite), washed with saturated aqueous sodium chloride (50 mL), dried (MgSO4), filtered and the solvent is evaporated off under reduced pressure to yield the crude product which is purified by column chromatography on silica gel, eluent ethyl acetate, and recrystallised from ethyl acetate-hexane to give the title compound as a yellow crystalline solid, m.p. 213-2150C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07557105B2 |
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| 출처 데이터셋 | uspto-grants-2009_07 |
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| ORD ID | ord-56d4ff03fd554ab5ade9deb49f7d226d |
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| 출처 메모 | uspto-grants-2009_07 |
|---|