참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Butyl bromide | HCID 8002 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Methyl 8-iodo-3-oxo-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylate | HCID 21086219 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Methyl 4-butyl-8-iodo-3-oxo-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylate | HCID 21086204 | 72.6% |
반응 단계
To a solution of Methyl 8-iodo-3-oxo-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylate (2.64 g) and potassium carbonate (5 g) in DMSO (20 mL) was added bromobutane (5 g), and the reaction mixture was stirred for 1 h at 80° C. The mixture was cooled to room temperature, diluted with 1:1 ethyl acetate/hexanes (100 mL) and water (160 mL), and separated. The organic layer was washed with water, and brine, dried (magnesium sulfate), filtered, and concentrated under reduced pressure. Purification by flash column chromatography (silica, 1:10 ethyl acetate/hexanes) afforded 2.24 g of the title compound: 1H NMR (300 MHz, CDCl3) δ 8.13, 7.63, 4.74, 3.96, 3.92, 1.64, 1.42, 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-8bfa03f2629947919ce80c51d962cc90 |
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| 출처 메모 | uspto-grants-2010_06 |
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