참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Butylamine | HCID 8007 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Binap, (A+-)- | HCID 634876 | — |
| 반응물 | Methyl 3,5-dibromo-4-methoxybenzoate | HCID 21086155 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Methyl 3-bromo-5-(butylamino)-4-methoxybenzoate | HCID 21086160 | — |
반응 단계
To a stirred solution of Pd(OAc)2 (144 mg), BINAP (1.2 g), and cesium carbonate (8.4 g) in toluene (100 mL) was added butylamine (1.6 mL), and the mixture was heated at 80° C. for 15 min. A solution methyl 3,5-dibromo-4-methoxybenzoate (4.2 g) in toluene (30 mL) was added dropwise over 20 min. The mixture was refluxed overnight. The mixture was cooled to room temperature, filtered through diatomaceous earth, and concentrated under reduced pressure. Purification by flash column chromatography (silica, 1:9 ethyl acetate/hexanes) provided 3.5 g of the title compound: 1H NMR (300 MHz, CDCl3) δ 7.52, 7.19, 3.90, 3.88, 3.18, 1.66, 1.46, 0.97.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07727997B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-cb35870106e04ff18d5775ee15a2958c |
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| 출처 메모 | uspto-grants-2010_06 |
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