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Triethylamine → 3-Cyclopentyloxy-4-methoxybenzal hydantoin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Cyclopentyloxy-4-methoxybenzaldehyde | HCID 2735893 | — |
| 反応物 | Diethyl 5-hydantoylphosphonate | HCID 3516088 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-Cyclopentyloxy-4-methoxybenzal hydantoin | HCID 54350727 | 77.8% |
反応手順
To a stirred solution of diethyl 5-hydantoylphosphonate (10 g, 42.3 mmol) and triethylamine (5.70 g, 56 mmol), in dry acetonitrile (100 ml) at room temperature was added a solution of 3-cyclopentyloxy-4-methoxybenzaldehyde (8 g, 36.3 mmol) in dry acetonitrile (75 ml), dropwise over 30 minutes. The resulting mixture was stirred at room temperature overnight, after which volatiles were removed in vacuo. The residue was diluted with 0.05N HCl (120 ml) and the precipitate collected by filtration. Recrystallization of this material with methylene chloride/methanol/diethyl ether afforded the title compound as a pale yellow solid (8.54 g). m.p. 220-222° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05922751 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-8002a67f5d7b458289c408796d875a7e |
| 出典メモ | uspto-grants-1999_07 |