関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Theobromine | HCID 5429 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 9-Methanesulfonyl-1-nonene | HCID 23287936 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(8-Nonenyl)-3,7-dimethylxanthine | HCID 15230635 | — |
反応手順
Theobromine (1.98 g, 11 mmol) was added to a suspension of NaH (600 mg of a 50% mineral oil slurry, 12 mmol) in DMSO (15 ml). After 15 minutes, 9-methanesulfonyl-1-nonene, prepared according to the foregoing procedure (2.25 g, 11 mmol), was added and the reaction mixture stirred for 6 days at 25° C. The reaction mixture was poured into 60 ml of water and extracted with dichloromethane (3×50 ml). The organic portions were combined, dried with magnesium sulfate, and evaporated to give a dark oil. Chromatography over silica gel using an ethyl acetate eluant produced 810 mg of 1-(8-nonenyl)-3,7-dimethylxanthine, a colorless oil (26% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06133274 |
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| 出典データセット | uspto-grants-2000_10 |
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| ORD ID | ord-9e0999aa8400423b940ee5d9810686bf |
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| 出典メモ | uspto-grants-2000_10 |
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