참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitric Acid | HCID 944 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | 1-(4-(Benzyloxy)-3-methoxyphenyl)-cyclobutanecarbonitrile | HCID 92135508 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | HCID 101043616 | HCID 101043616 | 92% |
반응 단계
A solution of 1-(4-(benzyloxy)-3-methoxyphenyl)cyclobutanecarbonitrile (5 g, 17.04 mmol), from Step 1, in acetic acid (20 mL)/acetic anhydride (20 mL) was cooled in an ice bath to 0° C. and treated slowly with 65% nitric acid (2.54 mL, 34.1 mmol). The reaction was stirred at 0° C. for 20 min, poured into ice and extracted with EtOAc. Organic layer was washed with saturated aqueous NaHCO3 and water. Organic layer was dried (MgSO4), filtered and concentrated. Purification by flash chromatography (silica gel, 5-50% EtOAc/hexane) afforded 1-(4-(benzyloxy)-5-methoxy-2-nitrophenyl)cyclobutanecarbonitrile (5.29 g, 92%). MS (ESI) m/z 339 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09284272B2 |
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| 출처 데이터셋 | uspto-grants-2016_03 |
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| ORD ID | ord-386300b954d34cb0b5618c78ffab2b9d |
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| 출처 메모 | uspto-grants-2016_03 |
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