Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 63273생성일: 2026년 10월 23일
Water → 1,1-dimethylethyl 7-(3-{[(4-methyl-2-pyridinyl)methyl]oxy}-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate
https://huagongshe.com/ko/reaction/63273
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | tert-Butyl 7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,4,5-tetrahydro-3H-benzo[d]azepine-3-carboxylate | HCID 57505869 | — |
| 반응물 | 2-Bromo-3-{[(4-methyl-2-pyridinyl)methyl]oxy}pyridine | HCID 86670544 | — |
| 촉매 | Palladium Chloride | HCID 24290 | — |
| 촉매 | Ferrocene-1,1'-bis-(diphenylphosphine) | HCID 635956 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 생성물 | 1,1-dimethylethyl 7-(3-{[(4-methyl-2-pyridinyl)methyl]oxy}-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate | HCID 70665243 | — |
반응 단계
To a degassed mixture of 2-bromo-3-{[(4-methyl-2-pyridinyl)methyl]oxy}pyridine (2.83 g), 1,1-dimethylethyl 7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (4.54 g) and cesium carbonate (9.9 g) in dioxane:water (4:1, 40 ml) was added PdCl2.dppf (0.828 g). The reaction mixture was heated at 120° C. overnight. The reaction mixture was added to water and extraction was carried out with ethyl acetate. The organic layer was dried over sodium sulphate and the filtrate was concentrated in vacuo. The crude product was purified through silica, eluting with 0-40% ethyl acetate in hexane. Appropriate fractions were concentrated in vacuo to yield the title compound, 3.8 g (84%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09447074B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-6b515ef1666142fa88156e73db3e63be |
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| 출처 메모 | uspto-grants-2016_09 |
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