참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Guanidine Hydrochloride | HCID 5742 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Methyl 7-oxospiro[5.6]dodecane-8-carboxylate | HCID 57429461 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 178508871 | HCID 178508871 | — |
반응 단계
A mixture of guanidine hydrochloride (430 mg, 4.5 mmol), the product from Example 16B (430 mg, 1.8 mmol), and potassium carbonate (623 mg, 4.5 mmol) in DMF (8 mL) was heated at 100° C. for 16 hours. Then, the temperature was raised to 120° C. for 2 hours. The mixture was cooled to ambient temperature and filtered through a layer of diatomaceous earth, then the filter pad was washed with a small amount of DMF. The filtrate was concentrated under reduced pressure, and the residue was chromatographed on silica gel (10:45:45 MeOH/CH2Cl2/EtOAc, eluant) to provide the title compound as a white solid. 1H NMR (300 MHz, DMSO-d6) ppm 10.62 (s, 1 H), 6.04 (s, 2 H), 2.57-2.64 (m, 2 H), 1.93-2.05 (m, 2 H), 1.60-1.71 (m, 4 H), 1.35-1.57 (m, 9 H), 1.15-1.28 (m, 1 H). MS (DCI+) m/z 248 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08278313B2 |
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| 출처 데이터셋 | uspto-grants-2012_10 |
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| ORD ID | ord-20a112029c3144edba1b63335cd378cf |
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| 출처 메모 | uspto-grants-2012_10 |
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