関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tegafur | HCID 5386 | — |
| 反応物 | Palladium bromide (PdBr2) | HCID 83469 | — |
| 溶媒 | Ammonium Hydroxide | HCID 14923 | — |
| 生成物 | 5-Fluoro-1-(oxolan-2-yl)pyrimidine-2,4-dione;palladium | HCID 131722404 | — |
反応手順
Palladium dibromide (0.377 g) is dissolved in 30% aqueous ammonium hydroxide (50 g) in a 250-mL flask equipped with a magnetic stir bar. Deionized water (60 g) is added to the solution, followed by addition of TS-1 (30 g, 2.12 wt. % titanium) over a 5 minute period. The slurry is stirred at 23° C. for 0.5 hr, then the solvent is removed by rotoevaporation at 55° C. The solids are dried in a vacuum oven (1 torr) at 50° C. for 4 hrs. The catalyst (Catalyst 3) analyzed for 0.5 wt % palladium, 2.1 wt % titanium, 0.7 wt % bromine and 0.37 wt % nitrogen.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06194591B1 |
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| 出典データセット | uspto-grants-2001_02 |
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| ORD ID | ord-b3db126bc3874a5ea85930bc65e93aff |
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| 出典メモ | uspto-grants-2001_02 |
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