참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl Acrylate | HCID 8821 | — |
| 반응물 | 7-Bromo-1,3,3-trimethylindolin-2-one | HCID 66812879 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Ethyl (2E)-3-(1,3,3-trimethyl-2-oxo-2,3-dihydro-1H-indol-7-yl)acrylate | HCID 66812761 | — |
반응 단계
A mixture of 7-bromo-1,3,3-trimethyl-1,3-dihydro-2H-indol-2-one from Step A (112 mg, 0.44 mmol), ethyl acrylate (0.238 mL, 2.20 mmol), triethylamine (0.124 mL, 0.88 mmol), and (PPh3)4Pd (51 mg, 0.044 mmol) in DMF (1.5 mL) was heated at 180° C. in a microwave reactor for 4 h. The reaction mixture was partitioned between CH2Cl2 (50 mL) and saturated aqueous NaHCO3 (50 mL). The organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo. The crude mixture was purified by silica gel chromatography, eluting with a gradient of CH2Cl2:EtOAc—100:0 to 60:40, to give the title compound. MS: m/z=274 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08143266B2 |
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| 출처 데이터셋 | uspto-grants-2012_03 |
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| ORD ID | ord-72d7ba4ab98640278a65dd23d81e6c0a |
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| 출처 메모 | uspto-grants-2012_03 |
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