関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | 3-Nitro-p-tolualdehyde | HCID 1798998 | — |
| 反応物 | Furan-2-carboximidamide hydrochloride | HCID 12231049 | — |
| 反応物 | 3-Phenylpropyl 4-(2-(1-piperidinyl)ethoxy)acetoacetate | HCID 22005512 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 22005532 | HCID 22005532 | 0.9% |
反応手順
A mixture of 3-phenylpropyl 4-(2-(1-piperidinyl)ethoxy)acetoacetate (10.0 g, 28.78 mmol), 4-methyl-3-nitrobenzaldehyde (4.75 g, 28.78 mmol), 2-amidinofuran hydrochloride (4.20 g, 28.78 mmol), morpholine (3.75 ml, 43.17 mmol), acetic acid (3.29 ml, 57.56 mmol), and sodium sulfate (8.17 g, 57.56 mmol) was stirred in ethanol (50 ml) for 1 hour at room temperature and then heated to 50° C. for 7 days. The ethanol was removed in vacuo and ethyl acetate was added to the residue. The mixture was filtered and the filtrate was washed with water, sodium hydrogen carbonate solution and brine, dried and evaporated to yield an oil. The oil was further purified by flash chromatography and RP-HPLC (twice) to give the title compound (150 mg) as an oil. Electrospray MS m/z 587 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06218538B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-25ce43649d774d819074daa971a8dfd7 |
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| 出典メモ | uspto-grants-2001_04 |
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