化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Carbonate → 2-[4-(3-Chloro-2-methylpropoxy)phenyl]-3-oxa-1-azaspiro[4.5]dec-1-ene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-3-chloro-2-methylpropane | HCID 95566 | — |
| 反応物 | 4-(3-Oxa-1-azaspiro[4.5]dec-1-en-2-yl)phenol | HCID 135526534 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2-[4-(3-Chloro-2-methylpropoxy)phenyl]-3-oxa-1-azaspiro[4.5]dec-1-ene | HCID 11950912 | 100% |
反応手順
To a solution of 4-(3-oxa-1-azaspiro[4.5]dec-1-en-2-yl)phenol ax8 (0.5 g, 2.16 mmol, 1 eq) in acetone (30 ml) is added 1-bromo-3-chloro-2-methylpropane (0.25 ml, 2.16 mmol, 1 eq) and potassium carbonate (0.6 g, 4.32 mmol, 2 eq). The mixture is stirred at reflux for 13 days. The mixture is concentrated, taken up in dichloromethane and washed twice with a saturated aqueous solution of ammonium chloride. The organic layer is dried over magnesium sulfate and the solvent is removed under reduced pressure to afford 0.7 g of 2-[4-(3-chloro-2-methylpropoxy)phenyl]-3-oxa-1-azaspiro[4.5]dec-1-ene ax64 as a colorless oil. This crude product is used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863450B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-92e8e93ab0034f668ea2f096302813fb |
| 出典メモ | uspto-grants-2011_01 |