関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Adenine | HCID 190 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Diethyl phosphoric acid | HCID 5166299 | — |
| 反応物 | Bis(chloromethoxy)methane | HCID 14843538 | — |
| 反応物 | Chloromethoxy(diethoxyphosphinomethoxy)methane | HCID 57012807 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 9-[(Diethylphosphonomethoxy)methoxymethyl]adenine | HCID 14843541 | — |
反応手順
To a suspension of 60% sodium hydride in mineral oil (1.4 g, 34.5 mmol) in DMF (100 mL) was added adenine (4.7 g, 34.5 mmol) and the mixture was stirred at 80° C. for 1 hr. To the resulting yellow solution was added dropwise a solution of chloromethoxy(diethoxyphosphinomethoxy)methane [(prepared from diethylphosphate (4.4 mL, 34.5 mmol) and bis-(chloromethoxy)methane (25 g, 172 mmol)] in DMF (20 mL) under nitrogen. After stirring at 25° C. for 15 hr, volatiles were removed in vacuo, and the resulting oily residue was purified by silica gel column chromatography using CH2Cl2 /10% MeOH as eluent to obtain the title compound as a colorless oil: yield 6.0 g (50%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05688778 |
|---|
| 出典データセット | uspto-grants-1997_11 |
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| ORD ID | ord-443bc952954a435483323b8702add03f |
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| 出典メモ | uspto-grants-1997_11 |
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