関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(2-Chloroethoxy)propane | HCID 123506 | — |
| 反応物 | 7-Benzyl-3-propylxanthine | HCID 22007302 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-Benzyl-1-(2-propoxyethyl)-3-propylxanthine | HCID 22007305 | — |
反応手順
1.7 g (12.48 mmol) of potassium carbonate were added at 60° C. to a suspension of 2.2 g (7.8 mmol) of 7-benzyl-3-propylxanthine (prepared according to Example 4a) in 70 ml of dimethylformamide and the mixture was stirred at this temperature for one hour. 1.3 ml (10.14 mmol) of 2-propoxyethyl chloride were then added dropwise and the mixture was stirred at 80° C. for 10 hours. 1.2 ml of methanol and 14 ml of water were then added, and the mixture was allowed to stand overnight, treated with a further 70 ml of water and extracted three times using 84 ml of methyl tert-butyl ether each time. The combined organic phases were washed twice with 42 ml of water each time, dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, dichloromethae/methanol (19/0.1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06214992B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-2460697181e740868704adf624e8fff0 |
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| 出典メモ | uspto-grants-2001_04 |
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