化工社化工社 化学情報印刷レポート · 研究参考用
Water → 11-Benzyl-5-difluoromethoxy-11-aza-tricyclo[7.3.1.02,7]trideca-2(7),3,5-triene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chlorodifluoromethane | HCID 6372 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 11-Benzyl-11-aza-tricyclo[7.3.1.02,7]trideca-2(7),3,5-trien-5-ol | HCID 9921762 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 11-Benzyl-5-difluoromethoxy-11-aza-tricyclo[7.3.1.02,7]trideca-2(7),3,5-triene | HCID 10268385 | — |
反応手順
11-Benzyl-11-aza-tricyclo[7.3.1.02,7]trideca-2(7),3,5-trien-5-ol (572 mg, 2.05 mmol) was stirred in dioxane (5 mL) and H2O (1 mL) at reflux under a balloon of freon (HCF2Cl). To this was added 3N KOH dropwise so as to maintain a pH˜12. The consumption of starting material was monitored by TLC for over 2 hours. The reaction was cooled, diluted with H2O (40 mL) and extracted with EtOAc. The organic layer was washed with a sat. aq. Na2CO3 soln. (25 mL) and brine (25 mL), dried (MgSO2), filtered and concentrated to an oil (620 mg, 92%). GCMS m/e 329 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706702B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-27242166685745c097b855f63cda34c3 |
| 出典メモ | uspto-grants-2004_03 |