関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Guanidine | HCID 3520 | — |
| 反応物 | Guanidine Hydrochloride | HCID 5742 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 3-(7,8-Dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile | HCID 54373447 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine | HCID 12849772 | 42.8% |
反応手順
Guanidine hydrochloride (11.46 g, 0.12 mole) in methanol (25 mL) was added to sodium methoxide (6.55 g, 0.12 mole) in methanol (40 mL) and the resultant sodium chloride was filtered and washed with methanol (10 mL). The guanidine solution was added to 3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile (11.5 g, 0.04 mole) and the mixture heated at reflux for 2 hr. Cooling the mixture at 3° C. provided 5.38 g of yellow solid in two crops. HPLC assayed yield of 28.6%. A sample recrystallized from alcohol/water gave mp 232°-4° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04761475 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-817e59b075864a43ba1165743bca3c56 |
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| 出典メモ | uspto-grants-1988_08 |
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