참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Bromide | HCID 253877 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Tempo | HCID 2724126 | — |
| 반응물 | Sodium Hypochlorite | HCID 23665760 | — |
| 반응물 | 3-(3',5'-Difluorobiphenyl-4-yl)propanoic acid | HCID 67183618 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-(3',5'-Difluorobiphenyl-4-yl)propanal | HCID 86700982 | — |
반응 단계
To a stirred solution of the compound obtained from step d above (0.7 g) in dichloromethane (10 mL), 2,2,6,6,-tetramethylpiperidine N-oxyl (4.36 mg) and potassium bromide (33.32 mg) were added at 0° C. under nitrogen atmosphere. Sodium hypochlorite (6.5 mL, 4% solution) was added at pH 8-9 (maintained by adding aqueous sodium bicarbonate solution). The reaction was stirred for 20 minutes at 0° C. The organic layer was separated and the aqueous layer was extracted with dichloromethane. The combined organic layers were washed with saturated aqueous sodium bicarbonate solution, water, and brine. The organic layer was dried over anhydrous sodium sulphate, filtered, and concentrated under reduced pressure to afford the title compound (0.57 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846910B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-b764c0ac49c54c7991fc0f43d269c016 |
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| 출처 메모 | uspto-grants-2014_09 |
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