化工社化工社 化学情報印刷レポート · 研究参考用
Water → 3-allyl-2-(4-methoxybenzylthio)-3H-spiro[benzo[h]quinazoline-5,1'-cyclohexan]-4(6H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 4-Methoxybenzyl bromide | HCID 165021 | — |
| 反応物 | 3-allyl-2-thioxo-2,3-dihydro-1H-spiro[benzo[h]quinazoline-5,1'-cyclohexan]-4(6H)-one | HCID 718815 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-allyl-2-(4-methoxybenzylthio)-3H-spiro[benzo[h]quinazoline-5,1'-cyclohexan]-4(6H)-one | HCID 46870295 | — |
反応手順
A mixture of 3-allyl-2-thioxo-2,3-dihydro-1H-spiro[benzo[h]quinazoline-5,1′-cyclohexan]-4(6H)-one (5, 0.100 g, 0.295 mmol), paramethoxybenzyl bromide (0.047 ml, 0.325 mmol), potassium hydroxide (0.025 g, 0.443 mmol) in Ethanol (1.738 ml) was refluxed overnight. 1 ml of water was added to the cooled reaction and the mixture was extracted with EtOAc 2×. The combined organics were washed with brine, dried over sodium sulfate, filtered, and concentrated. 1H NMR (500 MHz, CDCl3) δ ppm 8.17, 7.39-7.24, 6.88, 5.93, 5.31-5.26, 4.68, 4.57, 3.82, 3.07, 2.61, 1.75-1.72, 1.60-1.53, 1.43-1.37; MS (EI) m/z 459 (M+1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08501722B2 |
| 出典データセット | uspto-grants-2013_08 |
| ORD ID | ord-5104e10784e44714bd91a151ad1d2ff7 |
| 出典メモ | uspto-grants-2013_08 |