関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Diethoxymethane | HCID 10024 | — |
| 反応物 | 3-Methylxanthine | HCID 70639 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-Ethoxymethyl-3-methylxanthine | HCID 13747684 | — |
反応手順
52.5 g (0.28 mol) of p-toluenesulfonyl chloride were initially introduced into 50 ml of dimethylformamide and 22.6 g (0.29 mol) of sodium acetate were introduced with stirring and ice-cooling. The mixture was subsequently stirred for one hour, treated with 39.1 g of formaldehyde diethyl acetal and again subsequently stirred for one hour. 41.5 g of 3-methylxanthine were then introduced and the reaction mixture was heated at 90° C. for 2 hours. After cooling to 10° C., the precipitated product was filtered off with suction, washed with a little dimethylformamide and washed with demineralized water until chloride-free. The crude product obtained was recrystallized from dimethylformamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728686 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-d7d7141538f0422c85b05b45f2b6979e |
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| 出典メモ | uspto-grants-1998_03 |
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