참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl 4-methoxyacetoacetate | HCID 123500 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 반응물 | 2-Fluoro-5-iodoaniline | HCID 25418460 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178496286 | HCID 178496286 | 87% |
반응 단계
To a suspension of 2-fluoro-5-iodoaniline (9.83 g, 41.5 mmol) in 6 M HCl aqueous solution (83.0 mL) was added a solution of NaNO2 (3.43 g, 49.8 mmol) in water (8.3 mL) at 0° C. To a suspension of methyl 4-methoxy-3-oxobutanoate (5.37 mL, 41.5 mmol) and NaOAc (124 g) in EtOH (70 mL) was added the above solution at 0° C. The mixture was stirred at 0° C. for 10 min. The precipitates were collected by filtration, washed with water, dissolved in EtOAc, washed with brine, dried over MgSO4, filtered and concentrated in vacuo to yield the title compound (14.2 g, 87% yield) as a red solid: 1H NMR (DMSO-d6, 300 MHz): δ ppm 3.31 (3H, s), 3.83 (3H, s), 4.64 (2H, s), 7.03-7.41 (1H, m), 7.43-7.66 (1H, m), 7.85-8.07 (1H, m), 12.20 (1H, brs).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08513251B2 |
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| 출처 데이터셋 | uspto-grants-2013_08 |
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| ORD ID | ord-04543525e77c43b7b8a892ddd0fe211d |
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| 출처 메모 | uspto-grants-2013_08 |
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