関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Glycine ethyl ester, hydrochloride | HCID 2723640 | — |
| 反応物 | 4-chloro-8-(cyclopentyloxy)-7-methoxy-2H-chromen-2-one | HCID 77174794 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | ethyl 2-(8-(cyclopentyloxy)-7-methoxy-2-oxo-2H-chromen-4-ylamino)acetate | HCID 24849429 | — |
反応手順
A mixture of 4-chloro-8-(cyclopentyloxy)-7-methoxy-2H-chromen-2-one (170 mg, 0.58 mmol, Example 7, Step 1), glycine ethyl ester•HCl (97 mg, 0.69 mmol), triethylamine (0.2 mL, 1.4 mmol), and ethanol (2 mL) was heated at 75° C. in a sealed vial for 30 h. The reaction was allowed to cool to rt, concentrated, and purified by silica gel chromatography (3:2→1:4; hexanes:ethyl acetate) to give ethyl 2-(8-(cyclopentyloxy)-7-methoxy-2-oxo-2H-chromen-4-ylamino)acetate: 1H NMR (400 MHz, DMSO-d6): δ 7.93 (t, 1H), 7.68 (d, 1H), 7.08 (d, 1H), 4.92 (s, 1H), 4.80 (m, 1H), 4.13 (q, 2H), 4.10 (d, 2H), 3.86 (s, 3H), 1.90-1.45 (m, 8H), 1.20 (t, 3H); MS (ESI): 361.9.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745646B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-9a88ae54ca854067930fc7f4ebbb20b0 |
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| 出典メモ | uspto-grants-2010_06 |
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