참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl 4-bromobenzoate | HCID 12081 | — |
| 반응물 | Dimethyl phenylphosphonite | HCID 76277 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Methyl 4-[methoxy(phenyl)phosphoryl]benzoate | HCID 57925936 | — |
반응 단계
From a related procedure (Helv. Chim. Acta, 2004, 87, 825) a mixture of methyl 4-bromobenzoate (676 mg, 3.14 mmol), anhydrous NiBr2 (34.3 mg, 0.157 mmol), and PhP(OMe)2 (0.500 mL, 3.14 mmol) was added to a pressure vessel and heated to 160° C. (oil bath temperature) for 2 h. The reaction was cooled, diluted with EtOAc and washed with water (3×), brine, dried (MgSO4) and concentrated to afford ˜800 mg of a clear, colorless oil that solidified upon standing. The product was purified by MPLC (15-50% EtOAc in CH2Cl2) to afford the requisite product: MS: cal'd 291 (MH+), exp 291 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07981874B2 |
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| 출처 데이터셋 | uspto-grants-2011_07 |
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| ORD ID | ord-3369c978849642729c86f4c672298b2b |
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| 출처 메모 | uspto-grants-2011_07 |
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