化工社化工社 化学情報印刷レポート · 研究参考用
Theobromine → 1-(7-Octenyl)-3,7-dimethylxanthine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Theobromine | HCID 5429 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 8-Bromooct-1-ene | HCID 75907 | — |
| 反応物 | 1-(7,8-Dihydroxyoctyl)-3,7-dimethylxanthine | HCID 9797334 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(7-Octenyl)-3,7-dimethylxanthine | HCID 15230634 | 97% |
反応手順
1-(7,8-Dihydroxyoctyl)-3,7-dimethylxanthine was used as an intermediate for the synthesis of inventive compound no. 1514 (example 12). To a suspension of sodium hydride (580 mg, 24.2 mmol) in dimethylsulfoxide (100 ml) was added theobromine (3.96 g, 22.0 mmol). After stirring for 30 min, 8-bromo-1-octene (3.96 g, 22 mmol) was added and the mixture was stirred for 16 hr. The mixture was poured into water (200 ml) and extracted with dichloromethane (3×50 ml). The combined organic layers were washed with saturated aqueous sodium chloride solution (50 ml), dried over sodium sulfate, and the solvent was evaporated under vacuum to give 1-(7-octenyl)-3,7-dimethylxanthine (6.22 g, 97% yield) as an oil which solidified upon standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06020337 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-4109590c10504166b19c4335e4749422 |
| 出典メモ | uspto-grants-2000_02 |